反应详情

A mixture of 1.13 g (4 mmol) of 2-(3-chloropropyl)-6,7-dimethoxy-1,2,3,4-tetrahydro-isoquinolin-1-one, 1.04 g (4.4 mmol) of N-methyl-2-(2-methyl-naphth-1-yl)-ethylamine hydrochloride and 1.5 ml of N-ethyl-diisopropylamine is refluxed for 2 hours. The excess N-ethyl-diisopropylamine is evaporated off in vacuo and the residue remaining is dissolved in a mixture of methylene chloride and 2 molar sodium hydroxide solution. The organic phase is separated, washed with water, dried over magnesium sulphate, evaporated down in vacuo and purified over a 150 g silica gel column (0.062-0.2 mm) with methylene chloride and then with increasing amounts of ethanol (up to 5%). The hydrochloride is precipitated from a solution in acetone with ethereal hydrochloric acid and then recrystallised from acetone.

1. temperatureis refluxed for 2 hours
2. customThe excess N-ethyl-diisopropylamine is evaporated off in vacuo
3. dissolutionthe residue remaining is dissolved in a mixture of methylene chloride and 2 molar sodium hydroxide solution
4. customThe organic phase is separated
5. washwashed with water
6. dry with materialdried over magnesium sulphate
7. customevaporated down in vacuo
8. custompurified over a 150 g silica gel column (0.062-0.2 mm) with methylene chloride
9. customThe hydrochloride is precipitated from a solution in acetone with ethereal hydrochloric acid
10. customrecrystallised from acetone