Реакция #1923

ord-cca8c52f7ba34625b95aa6d245498aa5

Уравнение реакции

CC(=O)Nc1cccc2c1C(=O)c1ccccc1CO2
1-acetamido-6,11-dihydrodibenz[b,e]oxepin-11-one
O=C([O-])O.[Na+]
sodium bicarbonate
Nc1cccc2c1C(=O)c1ccccc1CO2
1-amino-6,11-dihydrodibenz[b,e]oxepin-11-one
Выход 81.0%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated
  2. 2
    Температураunder reflux for 2 hours
  3. 3
    Экстракцияfollowed by extraction with ethyl acetate (25 ml)
  4. 4
    ПромывкаThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. 5
    Сушкаdried over anhydrous magnesium sulfate
  6. 6
    ФильтрацияAfter the drying agent was filtered off
  7. 7
    Концентрированиеthe organic layer was concentrated under reduced pressure

Методика

In concentrated hydrochloric acid (10 ml), 1-acetamido-6,11-dihydrodibenz[b,e]oxepin-11-one obtained in Reference Example 3(0.25 g, 0.94 mmol) was heated under reflux for 2 hours. The reaction mixture was poured into a saturated aqueous solution of sodium bicarbonate, followed by extraction with ethyl acetate (25 ml). The organic layer was washed with a saturated aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the organic layer was concentrated under reduced pressure to give 1-amino-6,11-dihydrodibenz[b,e]oxepin-11-one as a yellow solid (0.17 g, 81%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05726325uspto-grants-1998_03