Agents Napoleon Solo (American) and Illya Kuryakin (Russian) work for U.N.C.L.E., a secret intelligence service working under the auspices of the U.N. Their immediate superior is Mr. Waverly (British), and they operate out of a secret base beneath the streets of New York City, and accesses through several cover business such as Del Floria's Tailor Shop and the Masque Club. U.N.C.L.E.'s primary nemesis was THRUSH, an organization dedicated to taking over the world. Like U.N.C.L.E., THRUSH used up-to-date spy equipment and advanced technology to complete its conquest.
Solo and Illya protect Miranda Bryant, the wife of a presidential candidate, from a THRUSH plot to kidnap her, not realizing that she has already been kidnapped and replaced with a double Irina, an unwitting dupe of THRUSH. When they do catch on, the candidate, Senator Bryant and his aide Fairbanks, agree to play along but Fairbanks is the one behind the plot to put a THRUSH agent in the White House.
U.N.C.L.E. and Thrush agents compete to gain possession of a mind-reading device created by a magician who has been murdered by Thrush.
Solo gets an unwelcome young companion (Kurt Russell), a ten year old who wants Solo to marry his widowed mother, in his efforts to find the source of a deadly chemical that killed an entire Scottish village. In a race to find the source with General Yokura (Leonard Strong), Solo eventually uses a ring on the finger of a statue to pinpoint a cave where the deadly chemical has leaked from, but has to use his wits to escape when he is trapped there by Yokura and his men.
Waverly is poisoned, and taken to a hospital where he is subjected to the rays of a brain-altering machine by THRUSH agent Dr, Dabree (Elsa Lanchester) designed to make him ineffective without killing him. While investigating others who have suffered the same fate, Solo finds Cecille Bergstrom (Yvonne Craig) and together they try to unravel the mystery and save Waverly.
Solo and Illya devise a clever scheme to discredit a Balkan intelligence chief (Werner Klemperer) with a bogus secret gas. With the help of a bankrupt exterminator (William Shatner) and his wife, Illya poses as a fellow countryman and exploits the paranoia of the chief and his bumbling assistant (Leonard Nimoy).
In spoof of "My Fair Lady," Solo is recuperating from a fall into a Venice canal, Illya teams with Mark Slate to uncover Baroness Bibi de Chasseur, a THRUSH money courier who has contact with the treasurer of THRUSH. They recruit a barroom entertainer, Rosy Shlagenheimer, an exact double, to impersonate her. The switch is made, but in the confusion the Baroness makes another switch and poses as Rosy, then finds herself falling in love with Slate.
While in Italy investigating a THRUSH plan to divert the Gulf Stream with heavy water, Solo finds himself eluding THRUSH guards, and ends up hiding under the bed of Pia Monteri. Solo escapes a shotgun wedding, the family feels Pia's honor has been compromised, and the girl's American uncles retired Prohibition-era gangsters ""Fingers"" Stilletto, Enzo ""Pretty"" Stilletto, and Federico ""Feet"" Stilletto are called. At the island headquarters of Louis Strago, Illya is tortured by Strago's sadistic female assistant, Miss Diketon. Solo joins forces with the Stilletto brothers to try and rescue him.
THRUSH creates a double for Solo, and with the seductive aid of Serena (Senta Berger), Darius Two (Michael Evans) kidnaps Solo and substitutes the phony into U.N.C.L.E.'s efforts to transport the code to a secret new weapon. Illya and stewardess Sandy Wister (Sharon Farrell) eventually realize a switch has been made, and the real Solo escapes and in a climactic scene battles "himself".
When a rare postage stamp at an auction reveals that a former SS scientist, Professor Amadeus, is still alive and experimenting with the secret of "suspended animation," Solo and Illya enlist the aid of college students Terry Brent (Brook Bundy) and Chuck Boskirk (Burt Brinckerhoff) to beat THRUSH agent Angelique (Janine Gray) to Amadeus's lab, where Solo is captured so his blood can be used to revive the suspended body of the Fuhrer.
While investigating a THRUSH plot to sabotage space shots, Solo and Illya are incapacitated by a quartzite radiation projector. Waverly assigns new trainee April Dancer along with over the age of retirement agent Mark Slateto find the antidote and destroy the plan. April infiltrates the cosmetics company of THRUSH agent Arthur Caresse as a model, but she is uncovered by Caresse's sister Jean.
Prior to an important conference at U.N.C.L.E. headquarters, a bizarre series of events occurs revolving around a strange man Mr. Hemmingway (Richard Haydn) who keeps appearing and disappearing at will in the building. Solo and Illya learn that he has been placed there by Waverly to test the security system, but THRUSH also has an inside agent, Riley (Peter Haskell), who plants an exploding false tabletop on the conference table at the direction of Dr. Egret (Lee Meriwether). Solo has only a few minutes, before the conference is to begin, to try and find out who the infiltrator is.
Solo, while searching for a secret map in Nevada, swallows an amnesia capsule just before being captured. THRUSH agents Arum Tertunian and Longolius try to revive his memory with a seductive female agent, Mara, while Illya races to find him before he starts to remember.
Illya goes to find Thrush's vaporizing machine, but is captured by Sophie, the headstrong daughter of the local tribal chief, Sulador. in New York Solo convinces retiring THRUSH agent David Lewin that THRUSH intends to kill him, and elicits his help. Lewin and Solo are taken to the base in the desert, just as Illya leads the band of nomads, whose confidence he has gained, in an attack on the base.
Alexander (Rip Torn) a megalomaniac industrialist, plans to conquer the world like his namesake, Alexander the Great by breaking each of the ten commandments along the way. he has his henchman Parvix (David Sheiner) steal the army's ""will gas"" to help him do so, and Solo investigates. Solo encounters Tracey Alexander (Dorothy Provine), Alexander's ex-wife, who wants to tag along with Solo to get the money Alexander owes her. The trail leads Solo, Illya, and Tracey to a posh party at Alexander's, where Solo defeats him in a human chess game; to a tomb, where Alexander and his aide Dr. Kavon (David Opatoshu) leave Solo tied under a descending scimitar while Illya and Tracey are hanging over a bottomless pit with a candle burning their rope; To Alexander's farm in Virginia, where Illya is nearly cut in two by various farm implements.
In the Yucatan, THRUSH agent Walter Brach (Carroll O'Connor) brainwashes important people from many nations to be "time bombs" who will return to their jobs and do THRUSH's bidding. After eluding Brach's henchmen Chuke (Shuji J. Nozawa) and his leopards, Solo and housewife Chris Linnel (Joan O'Brien) enlist the aid of Mrs. Karda (Dovima), Brach's numerologist, to help them escape.
Visiting Berlin headquarters in preparation for a high level U.N.C.L.E. conference, ""Summit Five,"" Solo finds agent Heinz Newman (Don Chastin) mysteriously murdered. Illya goes to Berlin, as does Harry Beldon (Albert Dekker), one of Waverly's counterparts in Section 1. Beldon suspects that either Solo or Gerald Struthers (Lloyd Bochner) committed the murder, while Illya suspects Beldon's secretary Helga Deniken (Suzanne Cramer), but Beldon himself turns out to be the traitor, and he plans to kill Waverly at the conference.
When secret "File 40" documents turn up outside headquarters, Waverly assigns Solo and Illya to find out if George Donnell is a double agent. Carla Drosten is too anxious to accuse Donnell and Solo must use special "Waverly rings" to try and expose the real double agent.
THRUSH agent Elom tries to kidnap a geologist who has developed an earthquake activating machine, but mistakes debt-ridden salesman Buzz Conway for the scientist. Solo and Illya let THRUSH go on thinking Conway is the scientist, while Elom lets his attraction for THRUSH agent Narcissus Darling interfere with his judgment. Conway is captured, and Solo and Illya must rescue him and find the machine.
Solo is nearly killed by a superhuman, robotlike girl, Margo Hayward, one of an army of such devices invented by Dr. Pertwee for THRUSH. Illya joins up with Margo's ex-roommate, Andy Francis, and finds the laboratory, where a roomful of robots attack them.
Investigating the shipment of a tidal-wave machine by THRUSH, Illya ends up aboard a merchant vessel run by Captain Morton. Morton is obsessed with his past disgrace in a court martial, and the crew is on the verge of a mutiny, which Illya leads just as THRUSH arrives to take possession of the device.
Solo and Illya go to visit a Nazi war criminal in prison, Von Etske (Will Kulova), but find that he has escaped with the aid of a special thought controlling device. His escape was observed by photographer Terry Cook (Judy Carne). Von Erske is joining forces with Zorgon Gurnius (George Macready), a fellow former Nazi, to reactivate their wartime triumvirate. Illya intercept Nexor, and finds that he is his exact double. He decides to impersonate Nexor to foil the plan.
Squire G. Emory Partridge (George Sanders) kidnaps Illya and lures Solo to his manor in order to kill them off in his dungeon torture chamber in revenge for a past encounter. But Peggy Durance (Bonnie Franklin) helps them escape, with the unintended aid of Partridge's bumbling wife Edith (Jeanette Nolan).
U.N.C.L.E. must transport captured THRUSH official Egon Stryker (Ralph Taeger) from New York to Washington with THRUSH rescuing him. While Waverly takes a decoy along one route, Solo and Illya take the real Stryker. Or is it ? But in a mixup, Fran Parsons (Joanna Moore),a secretary on her lunch hour, gets handcuffed to Stryker and has to go along.
Solo investigates the curious death of an air force man in Iowa with scuba gear, and with the help of Jill Denison (Katherine Crawford) uncovers a plan by Clint Spinner (Slim Pickens) to steal a missile- plane from a secret base under a farm.
Solo and Illya go to Algiers to obtain a rare old book containing a THRUSH code from Pierrot La Mouche who has stolen it from his boss, Colonel Hamid. But La Mouche has a high price he wants U.N.C.L.E. to help him obtain Janine whom he is in love with.
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