反応 #684132

反応方程式

PHOSPHORUS PENTACHLORIDE

hydroxymethylbenzoyl sulfide

→

Chloromethylbenzoyl sulfide

溶媒

ETHER

反応条件

後処理

1. 1
   温度cooling with ice
2. 2
   workup.STIRRINGwhole stirred for 2 hours at room temperature
3. 3
   ろ過The solution is filtered
4. 4
   濃縮the filtrate concentrated at 0.01 mm and a bath temperature of 40° C
5. 5
   洗浄washed with cold aqueous NaNHCO3 solution
6. 6
   乾燥The organic phase is dried over Na2SO4
7. 7
   workup.DISTILLATIONdistilled 20 parts of chloromethylbenzoyl sulfide having a boiling point at 0.1 mm of 111° to 113° C
8. 8
   その他is obtained

実験手順

42 PARTS OF PHOSPHORUS PENTACHLORIDE IS COVERED WITH A LAYER OF ABSOLUTE ETHER. While stirring and cooling with ice, an ethereal solution of 33.6 parts of hydroxymethylbenzoyl sulfide is dripped in and the whole stirred for 2 hours at room temperature. The solution is filtered, the filtrate concentrated at 0.01 mm and a bath temperature of 40° C, the residue taken up in methylene chloride and washed with cold aqueous NaNHCO3 solution. The organic phase is dried over Na2SO4 and distilled 20 parts of chloromethylbenzoyl sulfide having a boiling point at 0.1 mm of 111° to 113° C is obtained.

出典