反应详情

t-butyl 5-(2-chlorophenyl)-1,2,3,6,7,9-hexahydro-2-oxo-1-(2-phenylethyl)-8H-pyrido[4′,3′:4.5]thieno[2,3-e]-1,4-diazepine-8-carboxylate (22 g, 41 mmol) is dissolved a 23° C. in 1,2-chloro ethane (320 ml). Meta-chloroperoxybenzoic acid at 85% (21.6 g, 0.1 mol) is added. Agitation is carried out for 24 hours at 23° C. then a solution of 5N sodium hydroxide (400 ml) is added. After decanting, the organic phase is washed with water, dried over magnesium sulphate, filtered and concentrated with a rotary evaporator. After purification by chromatography on a silica column (eluent: ethyl acetate-heptane: 50-50 to 80-20), the fractions containing only the product ae evaporated. The solid obtained is agitated in a mixture of solvents: isopropyl ether-isopentane (20-80). After filtration on frit and washing with isopentane, the desired product is obtained in the form of a white powder (5.9 g, 26%).

1. customAfter decanting
2. washthe organic phase is washed with water
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated with a rotary evaporator
6. customAfter purification by chromatography on a silica column (eluent: ethyl acetate-heptane: 50-50 to 80-20)
7. additionthe fractions containing only the product ae
8. customevaporated
9. customThe solid obtained
10. filtrationAfter filtration on frit
11. washwashing with isopentane