HRID1900886

反应详情

EQUATION

反应方程式

HRID 1900886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a similar manner to Example 1, starting material step (c), the product of step (c) (2.59 g) and 4-cyanobenzoyl isocyanate (1.29 g) in acetonitrile (100 ml total) were reacted to give, after stirring at ambient temperature for 1 hour and storage at 10° C. overnight, a solid, which was crystallised from isopropanol to give t-butyl (2S)-2-(n-butylsulphonylamino)-3-[4-[3-(4-cyanobenzoyl)ureido]phenyl]propionate (2.32 g) as a white solid: m.p. 171°-173° C.; NMR Spectrum (CDCl3) 0.90 (3H, t), 1.37 (2H, m), 1.49 (9H, s), 1.73 (2H, m), 2.90 (2H, t), 3.11 (2H, m), 4.31 (1H, m), 5.61 (1H, d), 7.19 (2H, d), 7.42 (2H, d), 7.83 (2H, d), 8.19 (2H, d), 9.92 (1H, br s), 10.78 (1H, br s); Mass Spectrum m/Z 529 (M+H)+.

WORKUP

后处理

  1. customto give
  2. customstorage at 10° C. overnight, a solid, which was crystallised from isopropanol