反応 #425357

反応方程式

chloromethyl chlorosulphate

di-tert-butyl hydrogen phosphate

sodium bicarbonate

hydrogen sulphate

→

product

収率 52.3%

Di-tert-butyl chloromethyl phosphate

収率 52.3%

溶媒

dichloromethane

dichloromethane

water

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture was stirred at room temperature for 15 min
2. 2
   workup.STIRRINGit was stirred for 10 min
3. 3
   その他The organic layer was separated
4. 4
   洗浄washed with brine
5. 5
   その他evaporated under reduced pressure

実験手順

To a well stirred suspension of di-tert-butyl hydrogen phosphate (4.7 g, 22.47 mmol) in water (186 ml) was added sodium bicarbonate (7.5 g, 89.52 mmol) followed by tetra-n-butylammomium hydrogen sulphate (760 mg, 2.238 mmol). The reaction mixture was stirred at room temperature for 15 min. To the reaction mixture was added dichloromethane (112 ml) at 0° C. and it was stirred for 10 min followed by the addition of chloromethyl chlorosulphate (4.4 g, 26.85 mmol) in dichloromethane (75 ml) at same temperature. The resultant mixture was vigorously stirred overnight at room temperature. The organic layer was separated, washed with brine and evaporated under reduced pressure to yield 3.04 g of product as pale yellow oil.

出典