HRID2231180

反应详情

EQUATION

反应方程式

HRID 2231180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a magnetically stirred solution of 22.3 g (0.1 mol) N-Cbz-D-alanine in 50 mls of dry dichloromethane containing 0.5 mls of concentrated sulfuric acid at 0° C., was added dropwise a 10 g (0.1 mol) sample of 1-methylcyclopentene in 50 mls of dichloromethane. After 5 days of stirring at room temperature, the mixture was heated to reflux for 4 hours, after which the reaction was cooled to room temperature, washed with 100 mls of saturated NaHCO3, 100 mls of water and dried over MgSO4. Filtration followed by evaporation of the solvent yielded 1.81 g of the product.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 4 hours
  3. temperatureafter which the reaction was cooled to room temperature
  4. washwashed with 100 mls of saturated NaHCO3, 100 mls of water
  5. dry with materialdried over MgSO4
  6. filtrationFiltration
  7. customfollowed by evaporation of the solvent