反応 #4932

反応方程式

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

pyrrolidine

sodium hydroxide

fumaric acid

→

2,3-Dihydro-4-methyl-2-[2-(1-pyrrolidinyl)ethyl]pyrido[3,2-f][1,4]-oxazepin-5(4H)-one fumarate

反応条件

後処理

1. 1
   温度The solution was cooled to room temperature
2. 2
   抽出The resulting solution was extracted with chloroform (3×30 ml)
3. 3
   濃縮concentrated in vacuo
4. 4
   workup.ADDITIONwas added
5. 5
   ろ過The solution was filtered hot
6. 6
   温度the filtrate cooled to 20° C. for several hours
7. 7
   その他The resulting crystals, 14 g (47.8%) were collected
8. 8
   その他recrystallized from isopropyl alcohol, m.p. 147°-149° C.

実験手順

A sample of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-one hydrochloride, 16 g (0.058 mole), was dissolved in 65 ml of pyrrolidine. The stirred solution was heated to 80° C. for 3 hr. The solution was cooled to room temperature and dilute sodium hydroxide solution (50 ml) was added. The resulting solution was extracted with chloroform (3×30 ml) and concentrated in vacuo. The residue was taken up in boiling isopropyl alcohol (500 ml/ and fumaric acid (9.2 g, 0.079 mole) was added. The solution was filtered hot and the filtrate cooled to 20° C. for several hours. The resulting crystals, 14 g (47.8%) were collected and recrystallized from isopropyl alcohol, m.p. 147°-149° C.

出典