반응 #4298

반응 방정식

2-diisopropylaminoethyl chloride hydrochloride

potassium phthalimide

→

white crystalline product

수율 62.3%

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

수율 62.3%

용매

dimethyl formamide

반응 조건

후처리

1. 1
   기타the residue was partitioned between chloroform and water
2. 2
   추출The chloroform layer was extracted with 10% sodium hydroxide
3. 3
   기타After drying
4. 4
   기타removal of solvent
5. 5
   기타a brown oil was obtained which
6. 6
   기타slowly crystallized
7. 7
   기타recrystallized from methanol/diethyl ether

실험 절차

A solution of 2-diisopropylaminoethyl chloride hydrochloride (40.0 g, 0.2 mole) and potassium phthalimide (74.0 g, 0.4 mole) as stirred overnight at 85° C. in 500 ml of dimethyl formamide. The reaction mixture was stirred to dryness on a rotary evaporator, and the residue was partitioned between chloroform and water. The chloroform layer was extracted with 10% sodium hydroxide. After drying and removal of solvent, a brown oil was obtained which slowly crystallized. A portion of the oil was converted to the hydrochloride salt and recrystallized from methanol/diethyl ether to give 4.18 g (62.3%) of white crystalline product, m.p. 209°-211° C.

출처