HRID55555

反应详情

EQUATION

反应方程式

HRID 55555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 21.45 g of N-carbobenzoxy-carbonyl-L-isoglutamine ethyl ester in 200 mL of dry tetrahydrofuran kept at 0° C. to -5° C. in an ice-bath 11.82 mL of pyridine is added. To the above solution 9.84 mL of trifluoroacetic anhydride in 100 mL of tetrahydrofuran is added dropwise at such a rate that the bath temperatue is maintained. The solution is stirred for 2 hours at this temperature. The solution is evaporated to dryness and the oil is dissolved in ethyl acetate. The organic layer is washed with 1.0 N hydrochloric acid and sterile water. The solution dried and evaporated in vacuo to give an oil to give 14.8 g of ethyl γ-(N-carbobenzoxy)amino-γ-cyanobutanoate, 17.

WORKUP

后处理

  1. customkept at 0° C. to -5° C. in an ice-bath
  2. temperatureis maintained
  3. customThe solution is evaporated to dryness
  4. dissolutionthe oil is dissolved in ethyl acetate
  5. washThe organic layer is washed with 1.0 N hydrochloric acid and sterile water
  6. customThe solution dried
  7. customevaporated in vacuo
  8. customto give an oil