HRID1092934

反应详情

EQUATION

反应方程式

HRID 1092934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of C3F7OCF2CF2CH2CH2I (300 g, 0.68 mol) and N-methyl-formamide (300 mL), was heated to 150° C. for 26 h. Then the reaction was cooled to 100° C., followed by the addition of water to separate the crude ester. Ethyl alcohol (77 mL) and p-toluene sulfonic acid (2.59 g) were added to the crude ester, and the reaction was stirred at 70° C. for 15 minutes. Then ethyl formate and ethyl alcohol were distilled out to give a crude product. The crude product was dissolved in ether, washed with aqueous sodium sulfite, water, and brine in turn, then dried over magnesium sulfate. The product was then distilled to give 199 g of C3F7OCF2CF2CH2CH2OH in 85% yield. The boiling point was 71˜73° C. at 40 mm Hg (5333 Pa).

WORKUP

后处理

  1. temperatureThen the reaction was cooled to 100° C.
  2. customto separate the crude ester
  3. additionEthyl alcohol (77 mL) and p-toluene sulfonic acid (2.59 g) were added to the crude ester
  4. distillationThen ethyl formate and ethyl alcohol were distilled out
  5. customto give a crude product
  6. washwashed with aqueous sodium sulfite, water, and brine in turn
  7. dry with materialdried over magnesium sulfate
  8. distillationThe product was then distilled