HRID839936

反应详情

EQUATION

反应方程式

HRID 839936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a mixture of 10 ml of water and 20 ml of ethyl acetate, 1.6 g of tyrosinol was dissolved. To the solution were added dropwise 2 g of 2-methylbenzyloxycarbonyl choride and 10 ml of an aqueous solution containing 1.3 g of sodium carbonate alternately with stirring while cooling with ice. After stirring for two hours at room temperature, the ethyl acetate layer was collected and washed with 5% hydrochloric acid and then with water. The layer was dried and concentrated to dryness. The residue was crystallized from ethyl acetate-petroleum either to give 2.2 g of N-(2-methylbenzyloxycarbonyl)-tyrosinol with a mp. 78°-81° C in a yield of 70%. Analysis, calculated for C18H21O4N C 68.55, H 6.72, N 4.44, found C 68.88, H 6.84, N 4.42.

WORKUP

后处理

  1. dissolutionwas dissolved
  2. temperaturewhile cooling with ice
  3. stirringAfter stirring for two hours at room temperature
  4. customthe ethyl acetate layer was collected
  5. washwashed with 5% hydrochloric acid
  6. customThe layer was dried
  7. concentrationconcentrated to dryness
  8. customThe residue was crystallized from ethyl acetate-petroleum