HRID220652

反应详情

EQUATION

反应方程式

HRID 220652 的结构方程式

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 and 321 μl (2.30 mmol) of triethylamine in 15 ml of dichloromethane was cooled to 0° C. and admixed with 189 μl (1.97 mmol) of ethyl chloroformate. The ice bath was removed and the mixture was stirred for a further 1 h. The volatile constituents were removed on a rotary evaporator and the residue was purified by preparative HPLC [Method 20]. The product fractions were combined and freed from the solvents on a rotary evaporator. The residue was dried in an HV. This gave 527 mg (85% of theory) of the title compound.

WORKUP

后处理

  1. customThe ice bath was removed
  2. customThe volatile constituents were removed on a rotary evaporator
  3. customthe residue was purified by preparative HPLC [Method 20]
  4. customfreed from the solvents on a rotary evaporator
  5. customThe residue was dried in an HV