反应详情

3.77 ml (40 mmol) of acetic anhydride are added dropwise to a stirred mixture of 5.19 g (20 mmol) of octahydro-4a-(3-hydroxyphenyl)-2-methyl-cis-6(2H)-isoquinoline (see Example 3), 3.22 ml (40 mmol) of pyridine and 20 ml of toluene at 5°. The mixture is then kept at 22° for 2 hours. 20 ml of water is added to the mixture at 5°, and the mixture is stirred for 30 minutes at 22°. 40 ml of methylene chloride are added. Whilst being stirred, the aqueous phase of the resultant twophase mixture is adjusted to pH 7 by the addition of 4 g of sodium carbonate. The aqueous phase is then separated and extracted with methylene chloride. The organic phases are washed with water, dried, concentrated by evaporation and dried in a high vacuum. The title compound is obtained as a viscous oil which is crystallized as the hydrogen fumarate from isopropanol; M.Pt. 194° (decomposition).

1. stirringWhilst being stirred
2. customThe aqueous phase is then separated
3. extractionextracted with methylene chloride
4. washThe organic phases are washed with water
5. customdried
6. concentrationconcentrated by evaporation
7. customdried in a high vacuum