Реакция #4963

Уравнение реакции

dimethylamine

2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepine-5(4H)-thione

→

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

Условия реакции

Обработка

1. 1
   ДругоеThe reaction flask was sealed tightly
2. 2
   ДругоеThe dimethylamine was evaporated at room temperature
3. 3
   Промывкаwashed twice with 1N hydroxide and once with water
4. 4
   Сушкаdried over sodium sulfate
5. 5
   Фильтрацияfiltered
6. 6
   Концентрированиеconcentrated by rotary evaporation
7. 7
   ДругоеApproximately 0.8 g of the crude solid residue was triturated with isopropyl/ether
8. 8
   Другоеto give the crystalline free base, m.p. 104°-109° C.

Методика

To 50 ml of freshly collected dimethylamine was added 4.25 g (0.014 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepine-5(4H)-thione. The reaction flask was sealed tightly and allowed to stand at room temperature for 6 days. The dimethylamine was evaporated at room temperature. The solid residue was taken up in methylene chloride, washed twice with 1N hydroxide and once with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. Approximately 0.8 g of the crude solid residue was triturated with isopropyl/ether to give the crystalline free base, m.p. 104°-109° C.

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