反应详情

A mixture of the compound of step (a) (50 g, 70 mmol), sodium hydroxide (8.40 g, 210 mmol) and 5% palladium on carbon catalyst (10 g) in toluene (450 ml) and water (150 ml) was hydrogenated at room temperature and 414 kPa (60 p.s.i.) for 24 hours. The reaction mixture was filtered through celite (trade mark) and the toluene layer separated and discarded. The aqueous layer was then washed with methylene chloride (2×75 ml) and toluene (2×75 ml) and then cooled to 0° C. whereupon sulphuric acid (10.3 g, 105 mmol) was added. After granulating at 0° C. for 1 hour the product was filtered, washed with water (60 ml) and dried under vacuum at 50° C. for 16 hours to give the title compound (20.5 g, 68%). The proton NMR data was identical to that obtained in Example 3(b).

1. customwas hydrogenated at room temperature
2. filtrationThe reaction mixture was filtered through celite (trade mark)
3. customthe toluene layer separated
4. washThe aqueous layer was then washed with methylene chloride (2×75 ml) and toluene (2×75 ml)
5. additionwas added
6. waitAfter granulating at 0° C. for 1 hour
7. filtrationthe product was filtered
8. washwashed with water (60 ml)
9. customdried under vacuum at 50° C. for 16 hours