HRID630671

反应详情

EQUATION

反应方程式

HRID 630671 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

456 mg (0.68 mmol) of the compound from example 2A was dissolved in 8 ml dichloromethane. 300 mg (0.68 mmol) N-Phenyl-S-trityl-L-cysteinamide, 0.12 ml (0.68 mmol) N,N-diisopropylethylamine and 260 mg (0.68 mmol) HATU were added. The reaction mixture was stirred at room temperature for 4 h. From the reaction mixture the solvent was removed under reduced pressure. The raw product was purified in two portions by preparative RP-HPLC on a C18 column with a water methanol gradient from 9/1 to 1/9. The product-containing fractions were combined and concentrated to dryness under reduced pressure. This gave 361 mg (0.37 mmol, 53% of theory) of the desired product.

WORKUP

后处理

  1. customFrom the reaction mixture the solvent was removed under reduced pressure
  2. customThe raw product was purified in two portions by preparative RP-HPLC on a C18 column with a water methanol gradient from 9/1 to 1/9
  3. concentrationconcentrated to dryness under reduced pressure