HRID2177405

反应详情

EQUATION

反应方程式

HRID 2177405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

Into a 25-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed ethyl 3-chloro-5-(4-methylcyclohex-1-en-1-yl)-1,2-thiazole-4-carboxylate (150 mg, 0.52 mmol, 1.00 equiv), toluene (3 mL). DIBAL-H (0.926 mL) was added dropwise at −78° C. with stirring. The resulting solution was allowed to warm to 20° C. and then stirred for 1 h. The reaction was then quenched by the addition of MeOH. The resulting mixture was concentrated under reduced pressure. The residue was applied to a silica gel column, eluting with ethyl acetate/petroleum ether (20:80), to afford 45 mg (35%) of [3-chloro-5-(4-methylcyclohex-1-en-1-yl)-1,2-thiazol-4-yl]methanol as colorless oil.

WORKUP

后处理

  1. customInto a 25-mL round-bottom flask purged
  2. temperaturemaintained with an inert atmosphere of nitrogen
  3. stirringstirred for 1 h
  4. customThe reaction was then quenched by the addition of MeOH
  5. concentrationThe resulting mixture was concentrated under reduced pressure
  6. washeluting with ethyl acetate/petroleum ether (20:80)