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温度

0 °C

A cooled (0° C.) slightly yellow solution of methyl 5-(2,3-dihydrobenzo[b][1,4]dioxin-5-yl)-5-(1,1-dimethylethylsulfinamido)pentanoate (160 mg; 0.43 mmol) in MeOH (2 ml) was treated dropwise with a solution of 4 M HCl in 1,4-dioxane (0.22 ml; 0.88 mmol). The resulting yellow mixture was further stirred at 0° C., under nitrogen, for 10 min., and then at rt for 1 h. The reaction mixture was then concentrated to dryness under reduced pressure and the yellow oily residue was further dried under HV to give the chlorhydrate salt of methyl 5-amino-5-(2,3-dihydrobenzo[b][1,4]dioxin-5-yl)pentanoate as a yellow solid. LC-MS (conditions A): tR=0.47 min.; [M+H]+: 266.11 g/mol.

1. waitat rt for 1 h
2. concentrationThe reaction mixture was then concentrated to dryness under reduced pressure
3. customthe yellow oily residue was further dried under HV