HRID217248

反应详情

EQUATION

反应方程式

HRID 217248 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

To a solution trans-(3-hydroxy-cyclobutyl)-acetic acid methyl ester (168 mg, 1.17 mmol) in DMF (1.5 mL) is added, NaH (60% in oil, 70 mg, 1.75 mmol) at 0° C. After stirring at 0° C. for 15 minutes, benzyl bromide (167 uL, 1.40 mmol) is added at 0° C. The mixture is stirred at room temperature for 2 hours and quenched with H2O. The mixture is extracted with dichloromethane, and the organic layer is concentrated under reduced pressure. The obtained residue is purified by silica gel column chromatography to give trans-(3-benzyloxy-cyclobutyl)-acetic acid methyl ester (110 mg, 40%); ESI-MS m/z 235 [M+1]+, retention time 1.97 min (condition A).

WORKUP

后处理

  1. customat 0° C
  2. stirringThe mixture is stirred at room temperature for 2 hours
  3. customquenched with H2O
  4. extractionThe mixture is extracted with dichloromethane
  5. concentrationthe organic layer is concentrated under reduced pressure
  6. customThe obtained residue is purified by silica gel column chromatography