HRID1597662

反应详情

EQUATION

反应方程式

HRID 1597662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a THF/water (5:3, 8 mL) solution of (S)α-amino4-phenyl-butyric acid (0.61 g, 0.0034 mol) and triethylamine (1 mL) at 10° C. was added dibenzofuran-2-sulfonyl chloride (1.0 g, 0.00375 mol) in one portion with stirring. The resulting solution was stirred at room temperature for 24 hours. The solution was then concentrated in vacuo and the residue redissolved in water (10 mL). This solution was cooled in an ice bath and then acidified with 1N HCl. An oil was deposited, which was then triturated with ethyl acetate and hexane to give the title product (0.54 g, 35%), Melting point=130-132° C.

WORKUP

后处理

  1. stirringThe resulting solution was stirred at room temperature for 24 hours
  2. concentrationThe solution was then concentrated in vacuo
  3. dissolutionthe residue redissolved in water (10 mL)
  4. temperatureThis solution was cooled in an ice bath
  5. customwhich was then triturated with ethyl acetate and hexane