Dimethylformamide → 4-{[2-(Methylsulfanyl)ethyl]sulfanyl}-2-nitroaniline
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]#N)=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].CN(C)C=O.[BH4-].[Na+].[CH3:21][S:22][CH2:23]CCl>O>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][CH2:21][S:22][CH3:23])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12]参加物
6
実験手順
5.85 G. of 1-amino-2-nitro-4-thiocyanatobenzene is treated in 20 ml. dimethylformamide under nitrogen at 20°-25° with 1.14 g. sodium borohydride. After 1 hour 10 ml. of methylthioethylchloride is added and the mixture stirred overnight, diluted with water and extracted with chloroform. The dried chloroform solution is passed through a silica gel column, then evaporated to dryness to afford 1-amino-2-nitro-4-methylthioethylthiobenzene.
後処理
- customat 20°-25°
- extractionextracted with chloroform
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-9509cb1308b84299b432ecf7f7bcbc7c
- 出典データセット
- uspto-grants-1976_11
- 特許番号
- US03993768
反応ノート
読み込み中…