Reaktion #4945

Reaktionsgleichung

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

dimethylamine

→

yellow crystals

Ausbeute 76.0%

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

Ausbeute 76.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled in an ice bath
2. 2
   SonstigeThe flask was sealed tightly
3. 3
   workup.WAITleft
4. 4
   SonstigeThe dimethylamine and methanol were removed by rotary evaporation (60° C.; 30 mm)
5. 5
   Waschenwashed with 3×50 ml dil sodium hydroxide
6. 6
   Trocknendried over anhydrous sodium sulfate
7. 7
   Filtrationfiltered
8. 8
   Einengenconcentrated 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

Vorschrift

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.

Quelle