反应详情

Dissolve 3-tert-butoxycarbonyl-7-chloro-6-(5-methoxycarbonyl-pyridin-2-ylmethylthio)-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine (1.86 g, 4.03 mmol) in methanol (25 mL). Add 1M aqueous lithium hydroxide (12 mL) and stir at ambient temperature overnight. Remove methanol in vacuo, and dilute the mixture with cold 0.5M aqueous HCl to pH 4. Add brine and extract three times with EtOAc. Dry over anhydrous Na2SO4, and concentrate in vacuo to give the title compound as an off-white solid (1.78 g, 95%). MS (APCI+) m/z 449 (M+H)+, 349 (M+H−Boc)+.

1. extractionAdd brine and extract three times with EtOAc
2. dry with materialDry over anhydrous Na2SO4
3. concentrationconcentrate in vacuo