反应详情

To a suspension of 2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (2.02 g, 10 mmol) in 1,2-dichloroethane (15 mL) was added phthalimidoacetyl chloride (2.24 g, 10 mmol),and the mixture was stirred for 15 minutes at room temperature. To the reaction mixture was added a saturated aqueous solution of sodium hydrogencarbonate (10 mL) to give precipitate, which was filtered off. The aqueous layer of the filtrate was seperated. The organic layer was washed with water, dried over magnesium sulfate and subjected to filtration. The filtrate was concentrated under reduced pressure. The concentrate was combined with the precipitate filtered previously, which was washed with methanol, followed by recrystallization from chloroform-methanol to give 2.42 g (yield 62%) of a cis-trans mixture (3:2). m.p. 293°-294° C.

1. customto give precipitate, which
2. filtrationwas filtered off
3. customThe aqueous layer of the filtrate was seperated
4. washThe organic layer was washed with water
5. dry with materialdried over magnesium sulfate
6. filtrationsubjected to filtration
7. concentrationThe filtrate was concentrated under reduced pressure
8. filtrationfiltered previously
9. washwhich was washed with methanol
10. customfollowed by recrystallization from chloroform-methanol