HRID1696336

反应详情

EQUATION

反应方程式

HRID 1696336 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-azido-6-methoxy-2,2-dimethyl-3,4-dihydronaphthalen-1(2H)-one (2.50 g, 10.2 mmol) in EtOH (100 mL) at RT was added palladium on carbon (1.08 g, 10.2 mmol) in two portions. A hydrogen balloon was affixed to the reaction flask and the head space above the solvent was purged with H2. After 5 hours, the solution was filtered through a plug of celite and concentrated to provide the crude product as an oil. The residue was purified by column chromatography 100% DCM to 50% (10% MeOH/DCM/1% NH4OH) to provide the title compound as a yellow oil (2.04 g, 91% yield). MS m/z: 220.2 (M+1).

WORKUP

后处理

  1. customthe head space above the solvent was purged with H2
  2. filtrationthe solution was filtered through a plug of celite and
  3. concentrationconcentrated
  4. customto provide the crude product as an oil
  5. customThe residue was purified by column chromatography 100% DCM to 50% (10% MeOH/DCM/1% NH4OH)