HRID220653

反应详情

EQUATION

反应方程式

HRID 220653 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 500 mg (1.64 mmol) of the compound from Example 101A in 15 ml of dichloromethane was admixed at 0° C. with 260 μl (3.29 mmol) of ethyl isocyanate. The ice bath was removed and the reaction mixture was stirred for a further 1 h. Then all of the volatile constituents were removed on a rotary evaporator. The residue was purified by preparative HPLC [Method 23]. The product fraction was freed from the solvent on a rotary evaporator. Drying of the residue in an HV gave 546 mg (89% of theory) of the title compound.

WORKUP

后处理

  1. customThe ice bath was removed
  2. customThen all of the volatile constituents were removed on a rotary evaporator
  3. customThe residue was purified by preparative HPLC [Method 23]
  4. customThe product fraction was freed from the solvent on a rotary evaporator
  5. customDrying of the residue in an HV