反应详情

A mixture of ethyl 9-(2,3-dichlorophenyl)-4-(t-butyloxycarbonyl)-1,1-dioxo-2,3,4,5,6,9-hexahydro-7-methylpyrido[2,3-f][1,4]thiazepine-8-carboxylate (2.45 g, 4.6 mmole) from Example 7, in ethyl acetate (150 mL) was cooled to 0° C. and saturated with gaseous hydrogen chloride. The mixture was warmed to room temperature. The reaction was then again chilled to 0° C. and shaken with 200 mL of cold 4 N NaOH. The aqueous layer was separated and extracted with 2×100 mL of chloroform. The ethyl acetate layer was dried with brine and the combined organic extracts were dried over Na2SO4. The solvents were evaporated under reduced pressure and the residue triturated with ether to give the product (1.86 g, 94% yield).

1. temperatureThe reaction was then again chilled to 0° C.
2. customThe aqueous layer was separated
3. extractionextracted with 2×100 mL of chloroform
4. dry with materialThe ethyl acetate layer was dried with brine
5. dry with materialthe combined organic extracts were dried over Na2SO4
6. customThe solvents were evaporated under reduced pressure
7. customthe residue triturated with ether