HRID41647

反应详情

EQUATION

反应方程式

HRID 41647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

A solution of 4-(4-methoxycarbonylthiophen-3-yl)-piperidine-1-carboxylic acid t-butyl ester (100 mg, 310 μmol, 1.0 eq.) in THF (5 mL) was combined with a solution of LiAlH4 (23 mg) under nitrogen. The resulting solution was stirred for 30 minutes while the temperature was maintained at 0-5° C. in an ice/salt bath. The reaction was then quenched by the addition of water (50 μL) and aqueous NaOH (150 μL). The solids were filtered and the filtrate was concentrated under vacuum. The residue was applied onto a silica gel column and eluted with EtOAc/PE (1:10) to yield the titled compound (50 mg) as a colorless oil. MS m/z: [M+H]+ calcd for C15H24NO3S, 298. found 298.

WORKUP

后处理

  1. customThe reaction was then quenched by the addition of water (50 μL) and aqueous NaOH (150 μL)
  2. filtrationThe solids were filtered
  3. concentrationthe filtrate was concentrated under vacuum
  4. washeluted with EtOAc/PE (1:10)