反应详情

A solution of 3,4-dihydroxyphenethylamine hydrochloride (2.17 g) and N-benzyloxycarbonylaminoacetaldehyde diethyl acetal (4.0 g) in a mixture of n-butyl alcohol (20 ml) and water (3.5 ml) was refluxed for 4.5 hours. After the reaction, the solvent was distilled off under reduced pressure. To the residue were added water (15 ml) and sodium acetate. A precipitating oil was separated from the aqueous layer and chloroform was added thereto. The mixture was allowed to stand to give crystals. The crystals were collected by filtration, washed with chloroform and recrystallized twice from a mixture of methanol and ether to give 1(N-benzyloxycarbonylaminomethyl)-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline acetate (1.2 g), mp 158° to 162° C. (dec).

1. temperaturewas refluxed for 4.5 hours
2. customAfter the reaction
3. distillationthe solvent was distilled off under reduced pressure
4. additionTo the residue were added water (15 ml) and sodium acetate
5. customA precipitating oil was separated from the aqueous layer and chloroform
6. additionwas added
7. customto give crystals
8. filtrationThe crystals were collected by filtration
9. washwashed with chloroform
10. customrecrystallized twice from a mixture of methanol and ether