Acetic Acid → 2-Amino-6-methylbenzothiazole
反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH2:11])=[S:10])=[CH:4][CH:3]=1.CC(O)=O.Br.CS(C)=O>CCOC(C)=O>[NH2:11][C:9]1[S:10][C:6]2[CH:7]=[C:2]([CH3:1])[CH:3]=[CH:4][C:5]=2[N:8]=1参加物
6
反応条件
- 温度
- 80 °C
実験手順
(4-Methylphenyl)thiourea (2 mmol) was added to AcOH (4 ml), and the suspension was heated to 80° C. To the solution formed was added 33% HBr in AcOH (4 mmol) followed by DMSO (2.1 mmol). After stirring at 80° C. for 1 h, the reaction mixture was cooled to 50° C., diluted with EtOAc (10 ml) and filtered. The product (as HBr-salt) was taken up in H2O (5 ml) and treated with 1M aq. NaHCO3 (2 ml). Stirring was continued for 0.2 h. The precipitated aminobenzothiazole was then filtered, washed with H2O (10 ml) and dried (16 h at 45° C./20 mb); yield 67%.
後処理
- customTo the solution formed
- temperaturethe reaction mixture was cooled to 50° C.
- filtrationfiltered
- additiontreated with 1M aq. NaHCO3 (2 ml)
- stirringStirring
- waitwas continued for 0.2 h
- filtrationThe precipitated aminobenzothiazole was then filtered
- washwashed with H2O (10 ml)
- customdried (16 h at 45° C./20 mb)
出典と根拠
- ORDレコード
- ord-2c38c04a2ff54f61871a1c6ab0095848
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07087761B2
反応ノート
読み込み中…