N,1-Dimethyl-3,3-diphenylpropylamine → 1,N-dimethyl-3,3-diphenylpropylamine hydrochloride

HRID 622732노트

반응식

HRID 622732 반응식
CC1NC(C)=C(C(OCC[Cl:26])=O)C(C2C=CC=C([N+]([O-])=O)C=2)C=1C(OC)=O.[CH3:28][CH:29]([NH:44][CH3:45])[CH2:30][CH:31]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1>C1(C)C=CC=CC=1.C(OCC)C>[ClH:26].[CH3:28][CH:29]([NH:44][CH3:45])[CH2:30][CH:31]([C:38]1[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1

참가 물질

5

반응물 2

HCID 122534N,1-Dimethyl-3,3-diphenylpropylamineHCID 30168882-Chloroethyl methyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate

생성물 1

HCID 700429241,N-dimethyl-3,3-diphenylpropylamine hydrochloride

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

실험 절차

A solution of 3.94 g of methyl 2-chloroethyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)-pyridine-3,5-dicarboxylate and 4.78 g of 1,N-dimethyl-3,3-diphenylpropylamine in 12 ml of toluene was refluxed under stirring for 25 hours. Upon completion of the reaction the mixture was diluted with diethyl ether and the 1,N-dimethyl-3,3-diphenylpropylamine hydrochloride formed was collected by filtration. The filtrate was then evaporated, and the crude product thus obtained was purified by repeated chromatography on silica gel, using first chloroform, then chloroform:ethyl acetate (85:15 by volume) and lastly ethyl acetate as eluent. The purified product was dissolved in methanol and ethanolic hydrogen chloride was added. The solution was filtered and evaporated to dryness. Repeated washings with warm diethyl ether:acetone (98:2 by volume) afforded 2.98 g of the title compound, m.p. 113°-120° C.

후처리

  1. customUpon completion of the reaction the mixture

출처 및 근거

ORD 기록
ord-42b4d4c3734b4de88ae98a4118330e83
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772621

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