تفاعل #334494

معادلة التفاعل

dimethylamine

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

dimethylamine

oxalic acid

→

2-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methylpyrido[3,4-f][1,4]oxazepin-5(4H)-one oxalate hydrate

المذيبات

isopropyl alcohol

water

ظروف التفاعل

المعالجة

1. 1
   أخرىto evaporate
2. 2
   workup.DISSOLUTIONThe residue was dissolved in chloroform
3. 3
   أخرىto remove excess dimethylamine
4. 4
   أخرىThe residue was partitioned between dilute sodium hydroxide and ethyl acetate
5. 5
   تركيزThe ethyl acetate solution was concentrated
6. 6
   workup.DISSOLUTIONto dissolve the salt
7. 7
   أخرىThe resulting crystals were recrystallized from the same solvent

الإجراء التجريبي

A solution of 5 g (0.02 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,4-f][1,4]oxazepin-5(4H)-one, in 25 ml of dimethylamine was placed in a sealed vessel and stirred for 72 hr. The vessel was opened and the excess dimethylamine allowed to evaporate. The residue was dissolved in chloroform and the solvent was stripped off in vacuo to remove excess dimethylamine. The residue was partitioned between dilute sodium hydroxide and ethyl acetate. The ethyl acetate solution was concentrated and the residue was treated with 3 g (0.033 mole) of oxalic acid in 50 ml of isopropyl alcohol and enough water to dissolve the salt while boiling. The resulting crystals were recrystallized from the same solvent. Yield of product was 5.3 g (60%), m.p. 179°-181° C.

المصدر