Réaction #4962

Équation de réaction

dimethylamine

2-(2-chloroethyl)-2,3-dihydro-4,8-dimethylpyrido[3,2-f]-1,4-oxazepin-5(4H)-one hydrate

fumaric acid

→

2-[2-(Dimethylamino)ethyl]-2,3-dihydro-4,8-dimethylpyrido[3,2-f][1,4]-oxazepin-5(4H)-one fumarate

Solvants

isopropyl alcohol

Conditions de réaction

Traitement

1. 1
   AutreThe reaction flask was sealed tightly
2. 2
   workup.WAITleft
3. 3
   AutreThe dimethylamine was evaporated in a stream of air
4. 4
   Lavagewashed twice with 1N sodium hydroxide and once with water
5. 5
   Séchagedried over sodium sulfate
6. 6
   Filtrationfiltered
7. 7
   Concentrationconcentrated by rotary evaporation

Mode opératoire

To 50 ml of freshly collected dimethylamine was added 5.0 g (0.020 mole) of 2-(2-chloroethyl)-2,3-dihydro-4,8-dimethylpyrido[3,2-f]-1,4-oxazepin-5(4H)-one hydrate [1:1]. The reaction flask was sealed tightly and left standing at room temperature for 3 days. The dimethylamine was evaporated in a stream of air. The residue was taken up in methylene chloride, washed twice with 1N sodium hydroxide and once with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The syrupy residue was treated with 2 equivalents of fumaric acid in isopropyl alcohol which yield 5.2 g (52%) of white crystals, m.p. 164°-165° C.

Source