2- phcnyl

In contrast to its reaction with methyllithium, jV,Af-diethyl-5-phcnyl-3//-azepin-2-amine (1) with butylithium undergoes 4,5-addition to give 4-butyl-A, V-diethyl-5-phenyl-4,5-dihydro-3/7-azepin-2-amine (2)38. 

Phcnyl-17/-l,4-benzodiazepin-2(37/)-one is nitrated at position 7 to give 15. The yield was... 

This thione was obtained in 87% yield by a modification229 in which a stirred cooled suspension of P2S5 (9.3 g, 42 mmol) in THF (170mL) under N2 was treated with 15% BuLi in hexane (50.4ml., 84 mmol) at 5-10 C. The mixture was stirred at 20 C for 1 h when a clear yellow solution resulted. 7-Chloro-5-phcnyl-l 7/-l,4-benzodiazcpin-2(37/)-one (21.64 g, 80 mmol) was added and the mixture was heated under reflux for 16h, cooled and the product was collected. b See ref 230. 

A mixture of 7-chloro-5-phcnyl-17/-l,4-benzodiazepin-2(3//)-one (271 g, 1.0 mol), P2S3 (242 g, 1.09 mol) and pyridine (2 L) was refluxed with stirring for 45 min. The resulting solution was cooled in an ice bath and poured slowly into ice-cold sat. brine (5 I.). The precipitated solid was collected, washed with H20, dried and dissolved in CH2C12. The solution was filtered through a bed of activated alumina and con-... 

Chloro-2-(methylsulfanyl)-5-phcnyl-3f/-l,4-bcnzodiazepine (34) Typical Procedure 228... 

Chloro-2-mcthoxy-5-phcnyl-3A/-l,4-bcnzodiazepine 4-Oxide (40a) Typical Procedure 235... 

Aldol Reaction of (4R,5,5)-3-(2-cliloro-l-oxoethyl)-4-inefliyl-5-phcnyl-l,3-oxazolidin-2-one Typical Procedure ... 

A mixture of 2.54 g (22.6 mmol) of potassium terl-butoxide and 100 mL of THF is chilled to — 78 °C. A solution of 3.41 g (22.6 mmol) of dimethyl (diazoinethyl)phosphonate in 6 mL of THF is added over 5 min. After an additional 5 min, 2.0 g (11.3 mmol) of (/ )-5-phcnyl-2-hexanone are added over 5 min. After 18 h at — 78 C (Caution vent ), the mixture is allowed to warm to r.t. The mixture is diluted with pentane, then extracted with five 100-mL portions of water. The organic layer is dried (Na2SO j and evaporated, and the residue purified by silica gel column chromatography (petroleum ether 60-80°C) to give the cyclopentene yield 2.56 g (66%) colorless oil. 

Anilino-5 phcnyl-I,3,4-oxadiazol (R = C6IIS)549 Beim Erhitzen von 1,46g (10,0 mmol) 5-Phenyl-tctrazol init 5 ml (40 mmol) Phenyl-isocyanat auf 140-150° werden in 1 h 245 ml Stickstoff freigesetzt. Nach Ab-destillieren des ubcrschiissigen Isocyanats i. Wasserstrahlvak. wird der farblose kristallinc Riickstand aus Elhanol umkristailisiert Ausbeute 2.17g (92%) Schmp. 210-212°. 

Pentenoate Ethyl 2.2-Difluoro-3-hydroxy-5-phcnyl- E10b2. 52 (F.duct)... 

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