HRID1193310

反应详情

EQUATION

反应方程式

HRID 1193310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-(4-Methoxybenzyl)-7,7-dimethyl-1,4-dioxaspiro[4.5]decan-8-amine (2.3 g, 7.54 mmol, 1 eq) was dissolved in MeOH (30 ml); Pd(OH)2 (690 mg) was added, and hydrogenation was carried out for 2 h at RT under balloon pressure (H2). After monitoring by thin-layer chromatography, the reaction mixture was filtered off over Celite and the filtrate was concentrated under reduced pressure. The crude product was purified by column chromatography (Alox neutral, 1% methanol in dichloromethane). The desired product was obtained in the form of a yellow oil. Yield: 72% (1.0 g, 5.41 mmol).

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered off over Celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe crude product was purified by column chromatography (Alox neutral, 1% methanol in dichloromethane)