HRID1433255

反应详情

EQUATION

反应方程式

HRID 1433255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

N-{2-(Benzyloxy)-5-[(1R)-2-[(7-{4-(benzyloxy)-3-[(1R)-3-(diisopropylamino)-1-phenylpropyl]phenoxy}heptyl)amino]-1-{[tert-butyl(dimethyl)silyl]oxy}ethyl]phenyl}methanesulfonamide (Preparation 19, 96 mg, 0.10 mmol) and palladium hydroxide (20% by weight on carbon, 25 mg, 0.04 mmol) were dissolved in ethanol (3 ml), then ammonium formate (69 mg, 1.1 mmol) was added and heated to 80° C. for 1 hour. The reaction was cooled to room temperature and the mixture was filtered through Arbocel™ and the solvent removed in vacuo. The residue was dissolved in dichloromethane (containing a trace of methanol) and washed with water (brine was added to aid in the separation), the organic layer was dried (magnesium sulphate), filtered, and the solvents removed in vacuo to yield the title compound as a white foam, 68 mg.

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationthe mixture was filtered through Arbocel™
  3. customthe solvent removed in vacuo
  4. dissolutionThe residue was dissolved in dichloromethane (
  5. additioncontaining a trace of methanol) and
  6. washwashed with water (brine
  7. additionwas added to aid in the separation), the organic layer
  8. dry with materialwas dried (magnesium sulphate)
  9. filtrationfiltered
  10. customthe solvents removed in vacuo