HRID1966146

反应详情

EQUATION

反应方程式

HRID 1966146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a mixture of 3-methylenecyclobutanecarbonitrile (1.00 g, 0.0107 mol) in tetrahydrofuran (40 mL, 0.5 mol) was added 2.00 M of lithium diisopropylamide in tetrahydrofuran (6.44 mL) at −78° C. After stirred at −78° C. for 30 min, to the resulting mixture was added chloromethyl methyl ether (1.02 mL, 0.0134 mol). The reaction was stirred at −78° C. for 30 min, then allowed to warm up to rt, quenched with ammonium chloride, then extracted with ether. The combined organic layers were washed with water, brine, dried, and evaporated to dryness. The crude residue was used directly in next step.

WORKUP

后处理

  1. stirringThe reaction was stirred at −78° C. for 30 min
  2. temperatureto warm up to rt
  3. customquenched with ammonium chloride
  4. extractionextracted with ether
  5. washThe combined organic layers were washed with water, brine
  6. customdried
  7. customevaporated to dryness