Реакция #4945

Уравнение реакции

2-(2-chloroethyl)-2,3-dihydro-2,4-dimethylpyrido[3,2-f]-1,4-oxazepine-5(4H)-thione

dimethylamine

→

yellow crystals

Выход 76.0%

2-[2-(Dimethylamino)ethyl]-2,3-dihydro-2,4-dimethylpyrido[3,2-f][1,4]oxazepine-5(4H)-thione monohydrochloride

Выход 76.0%

Растворители

methanol

Условия реакции

Обработка

1. 1
   Температураcooled in an ice bath
2. 2
   ДругоеThe flask was sealed tightly
3. 3
   workup.WAITleft
4. 4
   ДругоеThe dimethylamine and methanol were removed by rotary evaporation (60° C.; 30 mm)
5. 5
   Промывкаwashed with 3×50 ml dil sodium hydroxide
6. 6
   Сушкаdried over anhydrous sodium sulfate
7. 7
   Фильтрацияfiltered
8. 8
   Концентрированиеconcentrated by rotary evaporation (70° C.; 30 mm)
9. 9
   workup.DISSOLUTIONThe crude oil was dissolved in isopropyl alcohol
10. 10
    workup.ADDITIONtreated with ethereal hydrogen chloride, which

Методика

To a suspension of 4.5 g (0.017 mole) of 2-(2-chloroethyl)-2,3-dihydro-2,4-dimethylpyrido[3,2-f]-1,4-oxazepine-5(4H)-thione in 20 ml of methanol, cooled in an ice bath, was added 40 ml of dimethylamine. The flask was sealed tightly and left standing at room temperature for 10 days. The dimethylamine and methanol were removed by rotary evaporation (60° C.; 30 mm). The residue was taken up in 150 ml of chloroform, washed with 3×50 ml dil sodium hydroxide, dried over anhydrous sodium sulfate, filtered and concentrated by rotary evaporation (70° C.; 30 mm). The crude oil was dissolved in isopropyl alcohol and treated with ethereal hydrogen chloride, which yielded 4.0 g (76%) of yellow crystals, m.p. 255° C. with decomposition.

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