Methanethiol → 3-(Methylsulfanyl)-4-nitroaniline
反応式
CN(C)C=O.C(=O)([O-])[O-].[K+].[K+].[CH3:12][SH:13].Cl[C:15]1[CH:16]=[C:17]([CH:19]=[CH:20][C:21]=1[N+:22]([O-:24])=[O:23])[NH2:18]>O>[CH3:12][S:13][C:15]1[CH:16]=[C:17]([CH:19]=[CH:20][C:21]=1[N+:22]([O-:24])=[O:23])[NH2:18]参加物
6
実験手順
A mixture of dry dimethylformamide (150 ml) and potassium carbonate (12.0 g) is stirred and methyl mercaptan is introduced as a gas for 45 minutes. After stirring for another 45 minutes, 3-chloro-4-nitroaniline (10.0 g) is added. The mixture is stirred and heated at 120°-130° C. for 18 hours. It is then cooled and poured into water (1 liter), the precipitate is collected and recrystallized from methanol to afford 8 grams of 3-methylthio-4-nitroaniline, m.p. 178°-182° C.
後処理
- stirringAfter stirring for another 45 minutes
- stirringThe mixture is stirred
- temperatureheated at 120°-130° C. for 18 hours
- temperatureIt is then cooled
- customthe precipitate is collected
- customrecrystallized from methanol
出典と根拠
- ORDレコード
- ord-a70badac2c44479e88ae62afe16bacac
- 出典データセット
- uspto-grants-1979_01
- 特許番号
- US04137310
反応ノート
読み込み中…