HRID575056

反应详情

EQUATION

反应方程式

HRID 575056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

This compound was prepared according to a procedure similar to that described in Procedure A. In a 100-mL 3-necked round-bottom flask, a solution of 1-(1-methylcyclopropyl)ethan-1-one (2 g, 20.38 mmol, 1.00 equiv) in tetrahydrofuran (5 mL) was added into a solution of bromo(ethynyl)magnesium (0.5 M in THF, 53 mL, 1.30 equiv) in tetrahydrofuran (5 mL). The resulting solution was stirred for 8 h at 0° C. in an ice/salt bath. The reaction was then quenched by the addition of 50 mL of sat. aq. NH4Cl. The resulting solution was extracted with 3×150 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 3×150 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 120 mg (5%) of 2-(1-methylcyclopropyl)but-3-yn-2-ol as colorless oil.

WORKUP

后处理

  1. customThis compound was prepared
  2. customThe reaction was then quenched by the addition of 50 mL of sat. aq. NH4Cl
  3. extractionThe resulting solution was extracted with 3×150 mL of ethyl acetate
  4. washThe resulting mixture was washed with 3×150 mL of brine
  5. dry with materialThe mixture was dried over anhydrous sodium sulfate
  6. concentrationconcentrated under vacuum
  7. customThis resulted in 120 mg (5%) of 2-(1-methylcyclopropyl)but-3-yn-2-ol as colorless oil