反応 #49740

反応方程式

t-butyl nitrite

3-amino-4-bromobenzotrifluoride

t-Butyl nitrite

3-amino-4-bromobenzotrifluoride

dimethyl disulphide

→

4-bromo-3-(methylsulphenyl)benzotrifluoride

溶媒

chloroform

chloroform

反応条件

後処理

1. 1
   温度The mixture was warmed until reaction
2. 2
   洗浄washed with water, hydrochloric acid (2M), water
3. 3
   乾燥dried (MgSO4)
4. 4
   ろ過filtered
5. 5
   その他The filtrate was evaporated to dryness
6. 6
   workup.DISTILLATIONthe residue was distilled

実験手順

t-Butyl nitrite (3 ml) was added to a mixture of 3-amino-4-bromobenzotrifluoride (4 g) and dimethyl disulphide (15 ml) in chloroform. The mixture was warmed until reaction started when t-butyl nitrite (11 ml) and a solution of 3-amino-4-bromobenzotrifluoride (16 g) in chloroform were added simultaneously. The resultant mixture was stirred for 24 hours, washed with water, hydrochloric acid (2M), water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 4-bromo-3-(methylsulphenyl)benzotrifluoride (16.4 g) as a yellow oil, b.p. 84°-88° C. at 2 mm Hg.

出典