HRID1369105

反应详情

EQUATION

反应方程式

HRID 1369105 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a suspension of 2-oxazoline (1.0 g, 11.5 mmol) in THF (40 mL) was added 60% NaH (460 mg, 11.5 mmol) and 3-bromopropyne (1. 0 mL, 11.2 mmol). The mixture was stirred for 1 h at 50° C. then for 3 h at 60° C., poured into aqueous 5% KHSO4, and extracted with ethyl acetate. The Organic layers were dried over MgSO4 and concentrated. The residue was purified by silica gel column chromatography with 1:1 hexane/ethyl acetate to give the title compound (1.02 g, 71%).

WORKUP

后处理

  1. waitfor 3 h at 60° C.
  2. extractionextracted with ethyl acetate
  3. dry with materialThe Organic layers were dried over MgSO4
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography with 1:1 hexane/ethyl acetate