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

HRID 622732ノート

反応式

HRID 622732 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  1. customUpon completion of the reaction the mixture

出典と根拠

ORDレコード
ord-42b4d4c3734b4de88ae98a4118330e83
出典データセット
uspto-grants-1988_09
特許番号
US04772621

反応ノート

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