HRID1729250

反应详情

EQUATION

反应方程式

HRID 1729250 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

33 mg of water-soluble carbodiimide hydrochloride was added under ice-cooling to a solution of 72 mg of 2-[[[N-(9-fluorenylcarbonyl)glycyl]-L-valyl]amino]-6-methylbenzoic acid in 3 ml of N,N-dimethylformamide. The mixture was stirred at 0° C. for 0.5 hour and, then, at room temperature for 18 hours. The mixture was concentrated to give a residue which was purified by a silica gel column chromatography (eluting solution: methylene chlorideether) to afford 60 mg of 2-[1(S)-[[N-(9-fluorenylcarbonyl)glycyl]amino]-2-methylpropyl]-5-methyl-4H-3,1-benzoxazin-4-one as a white powder (see Table 1).

WORKUP

后处理

  1. waitat room temperature for 18 hours
  2. concentrationThe mixture was concentrated
  3. customto give a residue which
  4. customwas purified by a silica gel column chromatography (eluting solution: methylene chlorideether)