反应 #4945

反应方程式

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

dimethylamine

→

yellow crystals

收率 76.0%

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

收率 76.0%

溶剂

methanol

反应条件

后处理

1. 1
   温度cooled in an ice bath
2. 2
   其他The flask was sealed tightly
3. 3
   workup.WAITleft
4. 4
   其他The dimethylamine and methanol were removed by rotary evaporation (60° C.; 30 mm)
5. 5
   洗涤washed with 3×50 ml dil sodium hydroxide
6. 6
   干燥dried over anhydrous sodium sulfate
7. 7
   过滤filtered
8. 8
   浓缩concentrated 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

实验过程

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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