反応 #4301

反応方程式

[(4-chlorobutyl)sulfonyl]benzene

isopropylamine

→

N-(1-Methylethyl)-4-(phenylsulfonyl)-1-butanamine hydrochloride

収率 30.0%

溶媒

chloroform

methanol

反応条件

後処理

1. 1
   その他The residue obtained
2. 2
   抽出the chloroform layer was extracted with water
3. 3
   乾燥The chloroform layer was dried
4. 4
   ろ過filtered
5. 5
   その他solvent removed
6. 6
   その他to give a dark brown oil
7. 7
   その他This salt was recrystallized from methanol-diethyl ether
8. 8
   その他dried in vacuo overnight at 80° C

実験手順

A solution of 105.95 g (0.456 mole) [(4-chlorobutyl)sulfonyl]benzene was heated overnight at 75° C. on an autoclave in 200 ml of isopropylamine. The reaction mixture was stripped to dryness. The residue obtained was dissolved in chloroform and the chloroform layer was extracted with water. The chloroform layer was dried, filtered, and solvent removed to give a dark brown oil. The oil was dissolved in methanol and converted to the hydrochloride salt. This salt was recrystallized from methanol-diethyl ether and dried in vacuo overnight at 80° C. This gave white crystalline product, m.p. 155°-157.5° C. in 30% yield.

出典