Реакция #334526

Уравнение реакции

2-[2-(dimethylamino)ethyl]-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepine-5(4H)-thione

hydrochloric acid

Ethyl alcohol

→

7-Amino-2-[2-(dimethylamino)ethyl]-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

Растворители

water

Условия реакции

Обработка

1. 1
   ТемператураThe reaction mixture was heated
2. 2
   Температураto reflux for 5 hr
3. 3
   ТемператураAfter cooling
4. 4
   ДругоеThe ethanol was removed by rotary evaporation at 70° C
5. 5
   ПромывкаThe remaining aqueous solution was washed with 3×100 ml of chloroform
6. 6
   Фильтрацияfiltered
7. 7
   Температураcooled with ice
8. 8
   ЭкстракцияThe aqueous was then extracted with 3×100 ml of chloroform
9. 9
   Сушкаdried over sodium sulfate
10. 10
    Фильтрацияfiltered
11. 11
    Концентрированиеconcentrated by rotary evaporation
12. 12
    ДругоеThe residue was crystallized from isopropyl alcohol
13. 13
    Другоеto give 3.5 g (55%) of yellow analytically pure crystals

Методика

To 7.0 g (0.023 mole) of 2-[2-(dimethylamino)ethyl]-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepine-5(4H)-thione was added 250 ml of 23% ammonium sulfide in water. Ethyl alcohol was added in amount sufficient to dissolve the starting compound (~50-60 ml). The reaction mixture was heated to reflux for 5 hr. After cooling, the reaction mixture was acidified with concentrated aqueous hydrochloric acid. The ethanol was removed by rotary evaporation at 70° C. The remaining aqueous solution was washed with 3×100 ml of chloroform, filtered, cooled with ice and made slightly basic with sodium hydroxide. The aqueous was then extracted with 3×100 ml of chloroform, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residue was crystallized from isopropyl alcohol to give 3.5 g (55%) of yellow analytically pure crystals.

Источник