反応 #1583874

反応方程式

3,3-diphenyl-1-propanol

triethylamine

isopropanol

MsCl

→

3,3-diphenylpropyl methanesulfonate

収率 73.3%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他was conducted at 25° C
2. 2
   その他After the completion of reaction
3. 3
   洗浄the reaction solution was washed with water thrice
4. 4
   乾燥The organic phase was dried over anhydrous sodium sulfate
5. 5
   その他evaporated
6. 6
   その他to remove the solvent
7. 7
   その他to produce an oily crude product
8. 8
   ろ過The resulting mixture was filtered by suction

実験手順

3,3-diphenyl-1-propanol (1000 g, 4.7 mol) was dissolved in 3 L dichloromethane. To the mixture was added triethylamine (712 g, 7.05 mol). After stirring at 0° C. for half an hour, to the resulting mixture was slowly added MsCl (645 g, 5.64 mol) dropwisely. The reaction was conducted at 25° C. After the completion of reaction monitored by TLC, the reaction solution was washed with water thrice. The organic phase was dried over anhydrous sodium sulfate, and evaporated to remove the solvent to produce an oily crude product. To the crude product was added isopropanol. The resulting mixture was filtered by suction to produce 3,3-diphenylpropyl methanesulfonate as a solid (1000 g) in a yield of 73% (two steps together).

出典