HRID483375

反应详情

EQUATION

反应方程式

HRID 483375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of sodium nitrite (4.6 g) in water (18 ml) was added dropwise at 0° C. over 20 minutes to a stirred mixture of p-nitrophenylalanine (6.3 g, Fluka) c.HCl (3.1 ml), 5% aqu. H2SO4 (80 ml) and water (10 ml). When addition was complete, the mixture was stirred at 0° C. for 1 hour, then allowed to warm to room temperature over 2 hours. The mixture was extracted with ethyl acetate (×4) and the extracts dried over MgSO4 and evaporated in vacuo to give the desired product as a white solid (3.1 g).

WORKUP

后处理

  1. additionWhen addition
  2. temperatureto warm to room temperature over 2 hours
  3. extractionThe mixture was extracted with ethyl acetate (×4)
  4. dry with materialthe extracts dried over MgSO4
  5. customevaporated in vacuo