HRID1380893

反应详情

EQUATION

反应方程式

HRID 1380893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Here, 1-[7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-on-3-yl]-3-[N-methyl-N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane (1.6 g, 0.0033 mol) is hydrogenated in glacial acetic acid (20 ml) in the presence of 10% palladium/charcoal (50 g) for 6 hours at 50° C. and at pressure (5 bar). The catalyst is removed by suction filtering, the glacial acetic acid is distilled off in vacuo and the residue is neutralized after the addition of water and potssium carbonate. The precipitate is suction filtered, washed with water to remove any salts and dried. The hydrochloride is precipitated from a solution in acetone using ethereal hydrohcloric acid. Yield: 1.2 g. Mp: 236°-238° C.

WORKUP

后处理

  1. customThe catalyst is removed by suction
  2. filtrationfiltering
  3. distillationthe glacial acetic acid is distilled off in vacuo
  4. additionafter the addition of water and potssium carbonate
  5. filtrationfiltered
  6. washwashed with water
  7. customto remove any salts
  8. customdried
  9. customThe hydrochloride is precipitated from a solution in acetone using ethereal hydrohcloric acid