HRID2186494

反应详情

EQUATION

反应方程式

HRID 2186494 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

In a 1 liter four-necked flask were charged 200 g (1.11 mol) of methyl (S)-3-hydroxy-3-phenylpropionate (optical purity: 87%e.e.), 77.8 g (1.56 mol) of hydrazine monohydrate, and 400 ml of methanol, and the mixture was heated at 70° C. for 3 hours. The reaction mixture was cooled to 5° C. with ice-water, followed by filtration. The collected crystals were dissolved in 4.7 liter of methanol while hot and cooled to 5° C. The crystals thus precipitated were collected by filtration and dried to give 148 g (74%) of the title compound. Melting point: 179.5° C. Optical purity: >99.9%e.e.

WORKUP

后处理

  1. filtrationfollowed by filtration
  2. dissolutionThe collected crystals were dissolved in 4.7 liter of methanol while hot and
  3. temperaturecooled to 5° C
  4. customThe crystals thus precipitated
  5. filtrationwere collected by filtration
  6. customdried