反応 #4299

反応方程式

dihydrochloride

2-[[N,N-bis(1-methylethyl)amino]ethyl]-2H-isoindole-1,3-dione

hydrazine hydrate

→

N,N-bis(1-Methylethyl)-1,2-ethanediamine, dihydrochloride

溶媒

methanol

ethanol

反応条件

後処理

1. 1
   温度at reflux for 5 hours
2. 2
   その他A white solid formed
3. 3
   濃縮The reaction mixture was concentrated almost to dryness on the rotary evaporator
4. 4
   workup.DISSOLUTIONThe residue was dissolved in chloroform
5. 5
   抽出extracted with 10% sodium hydroxide
6. 6
   その他After removing chloroform
7. 7
   その他a brown oil was obtained
8. 8
   その他After recrystallization from methanol-diethyl ether, 1.50 g (20%) of white crystalline product
9. 9
   その他m.p. 178°-182° C. (decomposition) was obtained

実験手順

A solution of 40.54 g (0.148 mole) of 2-[2-[[N,N-bis(1-methylethyl)amino]ethyl]-2H-isoindole-1,3-dione and hydrazine hydrate (85%, 11.8 g, 0.2 mole) in 400 ml of 95% ethanol was heated at reflux for 5 hours. The reaction mixture was allowed to cool to room temperature while standing overnight. A white solid formed. The reaction mixture was concentrated almost to dryness on the rotary evaporator. The residue was dissolved in chloroform and extracted with 10% sodium hydroxide. After removing chloroform, a brown oil was obtained. A portion of the oil was dissolved in methanol and converted to the dihydrochloride salt. After recrystallization from methanol-diethyl ether, 1.50 g (20%) of white crystalline product, m.p. 178°-182° C. (decomposition) was obtained.

出典