HRID15341

反应详情

EQUATION

反应方程式

HRID 15341 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1,1-dimethylethyl({(cis-1-[(3-fluoro-7-oxo-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-4-yl)methyl]-4-hydroxy-3-piperidinyl}methyl)carbamate (0.175 g, 0.405 mmol) in dichloromethane (2 ml) was treated with trifluoroacetic acid (1 ml) and stirred at room temperature for 20 min. The reaction mixture was evaporated and then redissolved using a 4:1 dichloromethane:methanol solution. The organic phase was then treated with aqueous sodium bicarbonate solution. The aqueous phase was extracted 10 times with a 4:1 dichloromethane:methanol solution and then the combined organic phases were dried and the solvent was removed under reduced pressure and the residue was subjected to column chromatography on silica gel using a dichloromethane, methanol and ammonia gradient to provide the desired compound (0.08 g).

WORKUP

后处理

  1. customThe reaction mixture was evaporated
  2. dissolutionredissolved
  3. additionThe organic phase was then treated with aqueous sodium bicarbonate solution
  4. extractionThe aqueous phase was extracted 10 times with a 4:1 dichloromethane
  5. dry with materialmethanol solution and then the combined organic phases were dried
  6. customthe solvent was removed under reduced pressure