HRID907279

反应详情

EQUATION

反应方程式

HRID 907279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of the product of step iii) (0.48 g) and N,N-dimethylethane-1,2-diamine (0.17 mL) in THF (20 mL) was added N,N-diisopropylethylamine (0.56 mL) followed by HATU (0.60 g) and the reaction stirred at room temperature for 3 hours. The reaction mixture was concentrated to dryness and the crude product purified by SiO2 chromatography (eluting with 90:10:0.1 dichloromethane:methanol:triethylamine). The fractions containing product were concentrated to dryness and the residue triturated with acetonitrile to give the title compound as a solid (0.35 g).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customthe crude product purified by SiO2 chromatography (eluting with 90:10:0.1 dichloromethane:methanol:triethylamine)
  3. additionThe fractions containing product
  4. concentrationwere concentrated to dryness
  5. customthe residue triturated with acetonitrile