Reaktion #4944

Reaktionsgleichung

2-(2-chloroethyl)-2,3-dihydro-2,4-dimethylpyrido[3,2-f]-1,4-oxazepin-5(4H)-one hydrochloride

dimethylamine

→

white crystals

Ausbeute 67.0%

2-[2-(Dimethylamino)ethyl]-2,3-dihydro-2,4-dimethylpyrido[3,2-f][1,4]oxazepin-5(4H)-one dihydrochloride

Ausbeute 67.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe flask was sealed tightly
2. 2
   workup.WAITleft
3. 3
   SonstigeThe methanol and dimethylamine were removed by rotary evaporation (70° C.; 30 mm)
4. 4
   Waschenwashed with 2×50 ml dil aqueous sodium hydroxide
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated by rotary evaporation (70° C.; 30 mm)
8. 8
   workup.ADDITIONThe syrupy residue was treated with hydrogen chloride in isopropyl alcohol, which

Vorschrift

To 4.5 g (0.015 mole) of 2-(2-chloroethyl)-2,3-dihydro-2,4-dimethylpyrido[3,2-f]-1,4-oxazepin-5(4H)-one hydrochloride in 15 ml of methanol was added 40 ml of dimethylamine. The flask was sealed tightly and left standing at room temperature for 8 days. The methanol and dimethylamine were removed by rotary evaporation (70° C.; 30 mm). The residue was taken up in 150 ml of chloroform, washed with 2×50 ml dil aqueous sodium hydroxide, dried over anhydrous sodium sulfate, filtered and concentrated by rotary evaporation (70° C.; 30 mm). The syrupy residue was treated with hydrogen chloride in isopropyl alcohol, which afforded 3.5 g (67%) of white crystals, m.p. 188°-90° C.

Quelle