반응 #4945

반응 방정식

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

dimethylamine

→

yellow crystals

수율 76.0%

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

수율 76.0%

용매

methanol

반응 조건

후처리

1. 1
   온도cooled in an ice bath
2. 2
   기타The flask was sealed tightly
3. 3
   workup.WAITleft
4. 4
   기타The dimethylamine and methanol were removed by rotary evaporation (60° C.; 30 mm)
5. 5
   세척washed with 3×50 ml dil sodium hydroxide
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   여과filtered
8. 8
   농축concentrated 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

실험 절차

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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