HRID1086602

反应详情

EQUATION

反应方程式

HRID 1086602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-[(1,1-dimethylethoxy)carbonyl]-2-[(phenylmethoxy)carbonyl]-2-methylhydrazine (15.0 g, 53. mmole) in 100 ml of methanol containing 4.9 ml of concentrated hydrochloric acid was hydrogenated at 1 atm in the presence of 3.0 g of 10% palladium-on-charcoal catalyst for 1 hour. The catalyst was filtered and the solvents were removed in vacuo. The residue was dissolved in water, the pH adjusted to 8.0 with sodium hydroxide and the mixture was extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and evaporated to give 5.6 g of the title compound as a colorless solid, m.p. 50° C.

WORKUP

后处理

  1. filtrationThe catalyst was filtered
  2. customthe solvents were removed in vacuo
  3. dissolutionThe residue was dissolved in water
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic phase was dried over magnesium sulfate
  6. customevaporated