反应详情

23.3 g sodium hydroxide in 218 mL water was added to 38 g 4-ethoxycarbonylmethyl-5-oxo-azepane-1,4-dicarboxylic acid 1-tert-butyl ester 4-ethyl ester in 155 mL THF. The reaction was stirred over night at RT, THF was removed and the mixture was extracted with dichlormethane. The aqueous part was acidified with 3M HCl to pH 3 at 0° C. The aqueous solution was extracted with dichloromethane, dried over magnesium sulfate, concentrated under reduced pressure to give 18.2 g of the desired product. (M+H)+=272

1. customTHF was removed
2. extractionthe mixture was extracted with dichlormethane
3. customwas acidified with 3M HCl to pH 3 at 0° C
4. extractionThe aqueous solution was extracted with dichloromethane
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure