반응 #4962

반응 방정식

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

용매

isopropyl alcohol

반응 조건

후처리

1. 1
   기타The reaction flask was sealed tightly
2. 2
   workup.WAITleft
3. 3
   기타The dimethylamine was evaporated in a stream of air
4. 4
   세척washed twice with 1N sodium hydroxide and once with water
5. 5
   건조dried over sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated by rotary evaporation

실험 절차

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.

출처