O-Xylene → 2H-1,5-Benzodiazepine-2-thione, 1,3-dihydro-4-phenyl-
反応式
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH2:7].C1(C)C(C)=CC=CC=1.[C:17]([CH2:25][C:26](S)=[S:27])(=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O1CCOCC1>O>[C:18]1([C:17]2[CH2:25][C:26](=[S:27])[NH:8][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=3[N:7]=2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1参加物
6
実験手順
A mixture of 1.08 g of o-phenylendiamine, 10 ml of xylene and 1.96 g of benzoyldithioacetic acid (Thuillier et al - Bull. Soc. Chim. Fr. 1938 (1959) is refluxed for 1 hour under a stream of nitrogen. The reaction may also be carried out in water, alcohol or dioxane. After cooling, the precipitate is filtered, washed with ethyl ether, and crystallized from ethyl acetate. Yield 2 g, m.p. 228°-230°C.
後処理
- temperature1938 (1959) is refluxed for 1 hour under a stream of nitrogen
- customThe reaction
- temperatureAfter cooling
- filtrationthe precipitate is filtered
- washwashed with ethyl ether
- customcrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-578e21f2f5b84458b25b5a8d1fbdf87a
- 出典データセット
- uspto-grants-1976_01
- 特許番号
- US03933793
反応ノート
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