反应详情

A mixture of 1-(N-benzyloxycarbonylaminomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrochloride (5.3 g), conc. hydrochloric acid (6 ml) and acetic acid (6 ml) was refluxed for 1 hour and 20 minutes. The reaction mixture was cooled and concentrated under reduced pressure. The residue was crystallized by adding methanol and acetone. The crystals were collected by filtration, washed with a mixture of methanol and acetone and recrystallized twice from a mixture of water, methanol and acetone to give 1-aminomethyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline dihydrochloride (1.2 g), mp 142° to 147° C. (dec).

1. temperaturewas refluxed for 1 hour and 20 minutes
2. temperatureThe reaction mixture was cooled
3. concentrationconcentrated under reduced pressure
4. customThe residue was crystallized
5. additionby adding methanol and acetone
6. filtrationThe crystals were collected by filtration
7. washwashed with a mixture of methanol and acetone
8. customrecrystallized twice from a mixture of water, methanol and acetone