反应详情

A solution of (R)-3-[5-(benzhydrylidene-amino)-2-fluoro-phenyl]-3-methyl-[1,4]oxazepan-5-one (338 mg, 0.84 mmol) in dioxane (5 ml) was treated with hydrochloric acid (1 N, 1.01 ml) at room temperature for 16 hours. For the workup, the reaction mixture was evaporated at reduced pressure, the resulting residue suspended in hydrochloric acid (1 N, 3 ml) and extracted with diethylether (2×10 ml). The combined organic layers were washed again with hydrochloric acid (1 N, 3 ml), then the aqueous layers were combined and evaporated at reduced pressure to yield the (R)-3-(5-amino-2-fluoro-phenyl)-3-methyl-[1,4]oxazepan-5-one hydrochloride (intermediate C13A) as a light brown foam (225 mg, 97% of theory) which was engaged in the next step without further purification. MS (ISP): m/z=239.3 [M+H]+.

1. customFor the workup, the reaction mixture was evaporated at reduced pressure
2. extractionextracted with diethylether (2×10 ml)
3. washThe combined organic layers were washed again with hydrochloric acid (1 N, 3 ml)
4. customevaporated at reduced pressure