HRID1038823

反应详情

EQUATION

反应方程式

HRID 1038823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a mixture of 1-tert-butyl 4-ethyl 4-methylpiperidine-1,4-dicarboxylate (0.10 g, 0.37 mmol) in THF (10 mL) and ethanol (20 mL) was added LiBH4 (0.032 g, 1.5 mmol). The mixture was stirred for about 8 h at rt. The mixture was diluted with water (20 mL) and extracted with EtOAc (3×20 mL). The EtOAc extracts were combined, dried over anhydrous Na2SO4, and concentrated in vacuo to give tert-butyl 4-(hydroxymethyl)-4-methylpiperidine-1-carboxylate (0.067 g, 80%): LC/MS (Table 2, Method i) Rt=0.29 min; MS m/z: 130 (M-Boc+H)+.

WORKUP

后处理

  1. extractionextracted with EtOAc (3×20 mL)
  2. dry with materialdried over anhydrous Na2SO4
  3. concentrationconcentrated in vacuo