反応 #1163178

反応方程式

DMSO

1-dodecanethiol

→

didodecyl disulfide

収率 90.0%

反応条件

後処理

1. 1
   温度was heated by a bath
2. 2
   温度The mixture was cooled
3. 3
   workup.STIRRINGwith stirring
4. 4
   その他to produce fine crystals
5. 5
   ろ過These were filtered off
6. 6
   洗浄rinsed with DMSO
7. 7
   その他Recrystallization from acetone

実験手順

A mixture of 9 ml of DMSO (127 mmole), 12 ml of 1-dodecanethiol (50 mmole), 0.1 ml of 37 percent hydrochloric acid (1.2 mmole), and 10.8 mg of iodine (0.085 mmole as HI) was heated by a bath, while stirring magnetically, at about 60°C. After one and a fourth hours, the lower phase became amber colored. The mixture was cooled with stirring to produce fine crystals. These were filtered off and rinsed with DMSO. Recrystallization from acetone gave 9.02 g of didodecyl disulfide (90 percent of theory). Mp, 33°-5°C. (reported, 33°-4°C.).

出典