HRID420778

反应详情

EQUATION

反应方程式

HRID 420778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of (2S)-benzyl-methyl-[5-(1,3,5-trimethyl-1 H-pyrazol-4-yl)-1,2,3,4-tetrahydro-naphthalen-2-yl]-amine (3.70 g, 10.291 mmol) in THF (20 mL) was added to Pd/C (1.20 g, 10% weight of Pd on activated carbon), and MeOH (120 mL) was added to the suspension. The reaction mixture was stirred under H2 overnight (ca. 16 h). It was filtered through Celite washing with AcOEt (2×100 mL) and the solvent was concentrated off to give 2.54 g of the methylamine as pale brown oil. The crude was purified by flash chromatography on silica gel (10-20-60% MeOH/CH2Cl2), to yield 2.05 g of the title product (Rf=0.3 (AcOEt/MeOH/Et3N 20:3:2), pale yellow coloured oil, 74% yield).

WORKUP

后处理

  1. additionwas added to the suspension
  2. filtrationIt was filtered through Celite
  3. washwashing with AcOEt (2×100 mL)
  4. concentrationthe solvent was concentrated off