HRID2046624

反应详情

EQUATION

反应方程式

HRID 2046624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-[(2S,3S)-2-methyl-1-[(1S)-1-phenylethyl]pyrrolidin-3-yl]propan-2-ol (2.00 g) synthesized by a known method, 10% palladium-carbon (50% water-containing product, 172 mg) and methanol (30 ml) was stirred under a hydrogen atmosphere at room temperature for 60 hr. The catalyst was removed by filtration through celite, and the mother liquor was concentrated. The obtained oily substance was dissolved in methanol, oxalic acid dihydrate (510 mg) was added thereto, and the mixture was concentrated. The residue was crystallized from diethyl ether to give the title compound (1.47 g, 1/2 hydrate).

WORKUP

后处理

  1. customThe catalyst was removed by filtration through celite
  2. concentrationthe mother liquor was concentrated
  3. dissolutionThe obtained oily substance was dissolved in methanol
  4. additionoxalic acid dihydrate (510 mg) was added
  5. concentrationthe mixture was concentrated
  6. customThe residue was crystallized from diethyl ether