反应详情

α-Amino-10,11-dihydro-5H-dibenzo[a,d]cycloheptene-5-acetic acid, hydrochloride (5.0 g, 16.5 mmol) is dissolved in 1N sodium hydroxide (70 mL) and 50 mL of water, cooled in an ice bath, and treated with acetic anhydride (2.3 mL, 25 mmol) keeping pH at 10 to 10.5. The mixture is stirred for an additional 20 minutes, then the pH is adjusted to 3 to 4 with concentrated hydrochloric acid. A precipitate is collected, washed with water, diethyl ether, and dried in a vacuum oven (50° C./10 mm Hg). The dried solid is recrystallized from ethyl acetate-hexane to give 2.41 g of the title compound; mp 220°-223° C.

1. customA precipitate is collected
2. washwashed with water, diethyl ether
3. customdried in a vacuum oven (50° C./10 mm Hg)
4. customThe dried solid is recrystallized from ethyl acetate-hexane