反应详情

The product from Step 11 (0.9 Kg, 1.53 mol) was dissolved in isopropanol (6.8 L) and water (1.04 L) and after purging with N2 10% Pd/C (90 g) and K2CO3 (0.212 Kg, 1.53 mol) were added and the suspension was hydrogenated for 60 to 70 mins under an 3 Barr pressure of H2. The solution was diluted with water (0.5 L) and filtered. To the filtrate was added aqueous HCl (30% hydrochloric acid, 0.85 Kg diluted with water 5.42 Kg) and the solution was concentrated at 60° C. under vacuum (removing 10 L isopropanol). Water (0.45 L) was added to the solution and concentration continued (until a further 10 L isopropanol had been removed). The aqueous phase was washed with EtOAc (4.61 L), diluted with acetonitrile (4.06 L) and netralised to pH 7.5-8.5 by addition of cone ammonia solution (0.35 Kg). The suspension was stirred for 2.5 h and then the solid was removed by filtration. The residue was washed with acetonitrile (2×0.8 L) and dried at 40° C. to constant weight to give the title compound 588 g (94% yield).

1. additionwere added
2. filtrationfiltered
3. additionTo the filtrate was added aqueous HCl (30% hydrochloric acid, 0.85 Kg diluted with water 5.42 Kg)
4. concentrationthe solution was concentrated at 60° C. under vacuum (removing 10 L isopropanol)
5. additionWater (0.45 L) was added to the solution and concentration
6. customhad been removed)
7. washThe aqueous phase was washed with EtOAc (4.61 L)
8. additiondiluted with acetonitrile (4.06 L) and netralised to pH 7.5-8.5 by addition of cone ammonia solution (0.35 Kg)
9. customthe solid was removed by filtration
10. washThe residue was washed with acetonitrile (2×0.8 L)
11. customdried at 40° C. to constant weight