反应详情

A solution of ethyl 4-[9-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-2,3-dihydro-1,4-benzoxazepin-4(5H)-yl]butanoate (Preparation 68) (61.7 g, 123 mmol) in ethanol (600 ml) was treated with 2M sodium hydroxide (123 ml, 247 mmol) and the mixture stirred at room temperature overnight. The solvent was evaporated and the residue dissolved in water (1 liter). The aqueous solution was cooled in ice/water and treated slowly with glacial acetic acid (28.3 ml, 494 mmol). The resulting gum was stirred vigorously until a filterable solid was obtained which was then collected by filtration and washed with more water (2×500 ml). After sucking the pad dry the material was dissolved in a 95:5 mixture of dichloromethane/methanol and dried (sodium sulphate). The solvent was removed by evaporation and the resulting solid was triturated under diethyl ether (200 ml), collected by filtration, washed with diethyl ether and dried to give the title compound as a colourless solid (54 g).

1. customThe solvent was evaporated
2. dissolutionthe residue dissolved in water (1 liter)
3. temperatureThe aqueous solution was cooled in ice/water
4. stirringThe resulting gum was stirred vigorously until a filterable solid
5. customwas obtained which
6. filtrationwas then collected by filtration
7. washwashed with more water (2×500 ml)
8. customdry the material
9. dissolutionwas dissolved in a 95:5 mixture of dichloromethane/methanol
10. dry with materialdried (sodium sulphate)
11. customThe solvent was removed by evaporation
12. customthe resulting solid was triturated under diethyl ether (200 ml)
13. filtrationcollected by filtration
14. washwashed with diethyl ether
15. customdried