反応 #343931

反応方程式

propargyl chloroformate

bis(4-hydroxyphenyl)methane

methylene chloride

trimethylamine

→

title compound

収率 93.6%

Bis(4-propargyloxycarbonyloxyphenyl)methane

収率 93.6%

溶媒

methylene chloride water

反応条件

後処理

1. 1
   その他A flask equipped with a stirrer
2. 2
   温度thermometer, nitrogen gas tube and reflux condenser
3. 3
   その他to react for 6 hours at 30° C
4. 4
   その他After the reaction
5. 5
   その他the organic phase was separated
6. 6
   乾燥by drying over magnesium sulfate overnight
7. 7
   ろ過After filtering
8. 8
   その他the filtrate was evaporated in a rotary evaporator
9. 9
   その他The resulting crystals were recrystallized

実験手順

A flask equipped with a stirrer, thermometer, nitrogen gas tube and reflux condenser was charged with 20.0 g of bis(4-hydroxyphenyl)methane, 50.0 g of methylene chloride and 23.0 g of trimethylamine. To the flask was added 26.0 g of propargyl chloroformate dropwise over one hour and the mixture was allowed to react for 6 hours at 30° C. After the reaction, the reaction mixture was treated with methylene chloride-water mixture and the organic phase was separated followed by drying over magnesium sulfate overnight. After filtering, the filtrate was evaporated in a rotary evaporator. The resulting crystals were recrystallized to give the title compound melting at 60° C. at a yield of 93.6% of theory.

出典