HRID477417

反应详情

EQUATION

反应方程式

HRID 477417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To the crude 1-chloro-3-decyloxy-2-propanol prepared as described above and cooled to 40° C. was added NaOH (50% aqueous, 76 g, 2.2 mole) and water (44 g). The temperature rose to 50° C., then the mixture was heated to 85°-90° C. for three hours. Analysis by GC showed the crude product contained 11% unreacted alcohol and 75% of the expected epoxide. Water (200 ml) was added to dissolve precipitated salt. The aqueous phase was separated (pH 4) and the organic phase washed with 5% NaCl solution to pH 7-8 (2×400 ml). The crude product (435 g, 102%) was fractionally distilled at 12 mmHg to yield 286 g of (decyloxy)methyloxirane (67% overall based on epichlorohydrin). GC showed the product was 97% pure.

WORKUP

后处理

  1. customrose to 50° C.
  2. temperaturethe mixture was heated to 85°-90° C. for three hours
  3. dissolutionto dissolve
  4. customprecipitated salt
  5. customThe aqueous phase was separated (pH 4)
  6. washthe organic phase washed with 5% NaCl solution to pH 7-8 (2×400 ml)
  7. distillationThe crude product (435 g, 102%) was fractionally distilled at 12 mmHg