HRID69160

反应详情

EQUATION

反应方程式

HRID 69160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride was added to a solution of (4-benzyloxy-phenyl)-[6-(1-methyl-1H-pyrazol-4-yl)-imidazo[1,2-b]pyridazin-3-yl]-methanone (Stage 5.2, 190 mg, 0.46 mmol) in ethanol (1.5 mL) and the reaction stirred for 16 h. Water was added to the reaction and the resulting solid was filtered off and dried under vacuum. The solid was dissolved in TFA (2 mL) and to this solution was added triethylsilane (0.18 mL, 1.16 mmol) and the mixture was stirred at rt for 30 min. Water was added and the mixture extracted with EtOAc. The EtOAc extract was dried, filtered and concentrated to give the title compound as red solid (tR 1.3 min (conditions 2), MH+=396).

WORKUP

后处理

  1. filtrationthe resulting solid was filtered off
  2. customdried under vacuum
  3. dissolutionThe solid was dissolved in TFA (2 mL) and to this solution
  4. stirringthe mixture was stirred at rt for 30 min
  5. extractionthe mixture extracted with EtOAc
  6. extractionThe EtOAc extract
  7. customwas dried
  8. filtrationfiltered
  9. concentrationconcentrated