HRID274078

反应详情

EQUATION

反应方程式

HRID 274078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 1-benzylaminomethyl-7-methoxy-1,2,3,4-tetrahydro-1-naphthalenol hydrochloride (45.00 g), ammonium formate (25.50 g), and 10% palladium on carbon (50% wet, 4.5 g) in methanol was refluxed for 40 minutes. After cooling, the catalyst was removed by filtration and the filtrate was evaporated in vacuo. Water (45 ml), 1N hydrochloric acid (90 ml) and diethyl ether (120 ml) were added to the residue and the aqueous layer was separated. The aqueous layer was made alkaline with 5N aqueous sodium hydroxide (45 ml), and extracted with ethyl acetate (600 ml×6 times). The organic layers were combined, dried over sodium sulfate, and evaporated in vacuo to give 1-aminomethyl-7-methoxy-1,2,3,4-tetrahydro-1-naphthalenol (27.89 g) as a pale yellow powder.

WORKUP

后处理

  1. temperaturewas refluxed for 40 minutes
  2. temperatureAfter cooling
  3. customthe catalyst was removed by filtration
  4. customthe filtrate was evaporated in vacuo
  5. additionWater (45 ml), 1N hydrochloric acid (90 ml) and diethyl ether (120 ml) were added to the residue
  6. customthe aqueous layer was separated
  7. extractionextracted with ethyl acetate (600 ml×6 times)
  8. dry with materialdried over sodium sulfate
  9. customevaporated in vacuo