反応式
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=[S:15])[N:7]([CH3:14])[CH2:8][CH:9]([CH2:11][CH2:12]Cl)[O:10][C:4]=2[CH:3]=1.[CH3:18][NH:19][CH3:20]>C(O)C.Cl>[ClH:1].[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=[S:15])[N:7]([CH3:14])[CH2:8][CH:9]([CH2:11][CH2:12][N:19]([CH3:20])[CH3:18])[O:10][C:4]=2[CH:3]=1参加物
実験手順
A solution of 9.8 g (0.04 mole) of 8-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione in 50 ml of absolute ethanol and 10 ml of a 40% aqueous solution of dimethylamine were mixed and heated in a steel bomb at 100° C. for 16 hr. The ethanol was evaporated under reduced pressure and the residue dissolved in chloroform and partitioned with 10% sodium hydroxide solution. The chloroform layer was evaporated under reduced pressure to give an amorphous solid. The solid was dissolved in 6N hydrochloric acid and the solution washed with ethyl acetate. The aqueous layer was basified with 50% sodium hydroxide and extracted with ethyl acetate. The ethyl acetate layer was evaporated under reduced pressure to give a viscous oil comprised substantially of the free base of the title compound which was dissolved in absolute ethanol and reacted with ethereal hydrogen chloride. The hydrochloride salt was recrystallized from ethanol to give 30 g (25%) product, m.p. 196°-199° C.
後処理
- customThe ethanol was evaporated under reduced pressure
- dissolutionthe residue dissolved in chloroform
- custompartitioned with 10% sodium hydroxide solution
- customThe chloroform layer was evaporated under reduced pressure
- customto give an amorphous solid
- washthe solution washed with ethyl acetate
- extractionextracted with ethyl acetate
- customThe ethyl acetate layer was evaporated under reduced pressure
- customto give a viscous oil
出典と根拠
- ORDレコード
- ord-b1a7ed0ed9204503b365a6200479ed5b
- 出典データセット
- uspto-grants-1987_11
- 特許番号
- US04705853
関連ノート
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