HRID1720820

反应详情

EQUATION

反应方程式

HRID 1720820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of phosphorus trichloride (19 mg) in pyridine (4 ml), 4-aminobenzoyl-glutamic acid di-t-butyl ester (106 mg) was added, followed by stirring at room temperature for 1 hour. To this mixture, 6,7-bis(octadecylcarbamoyloxy)-4-thiaheptanoic acid as obtained in Reference Example 10 (216 mg) was added, followed by stirring at 50° C. for 1 hour. After solvent concentration under reduced pressure, the resulting residue was purified by silica gel preparative TLC (dichloromethane:methanol=50:1×3) to yield the title compound (102 mg, yield 32%) as a colorless solid.

WORKUP

后处理

  1. additionwas added
  2. stirringby stirring at 50° C. for 1 hour
  3. concentrationAfter solvent concentration under reduced pressure
  4. customthe resulting residue was purified by silica gel preparative TLC (dichloromethane:methanol=50:1×3)