HRID1765972

反应详情

EQUATION

反应方程式

HRID 1765972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
64 °C

PROCEDURE

实验过程

A four-necked 500 mL round bottom flask was equipped with a mechanical stirrer, nitrogen inlet, condenser and thermometer. It was charged with 17.8 grams (0.10 moles) of 2,6-diisopropylphenol, 200 mL of THF, 8.0 grams (0.20 mole) of sodium hydroxide pellets, and 387 grams (3.0 moles, 194 mL) of bromochloromethane. The reaction mixture was heated to 64° C. and held for 2-3 hours until no more 2,6-diisopropylphenol was present as measured by GC. After cooling to 25° C., the suspension was filtered and the filter cake was washed with THF. The THF was removed by rotary evaporation and the resultant oil was distilled under vacuum (0-1 torr, b.p.=80° C.) to give 16.9 grams (0.074 moles, 75% yield) of O-chloromethyl 2,6-diisopropyl phenol.

WORKUP

后处理

  1. customA four-necked 500 mL round bottom flask was equipped with a mechanical stirrer, nitrogen inlet, condenser
  2. temperatureAfter cooling to 25° C.
  3. filtrationthe suspension was filtered
  4. washthe filter cake was washed with THF
  5. customThe THF was removed by rotary evaporation
  6. distillationthe resultant oil was distilled under vacuum (0-1 torr, b.p.=80° C.)