N,N-Diethylethylenediamine → HCID 21486957, 화합물

HRID 1414278노트

반응식

HRID 1414278 반응식
[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][NH2:6])[CH3:2].[CH3:9][O:10][C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][C:20]=1[O:21][CH3:22])[CH:17]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[N:16]([C:29](Cl)=[O:30])[CH2:15][CH2:14]2>O>[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][NH:6][C:29]([N:16]1[CH2:15][CH2:14][C:13]2[C:18](=[CH:19][C:20]([O:21][CH3:22])=[C:11]([O:10][CH3:9])[CH:12]=2)[CH:17]1[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:30])[CH3:2]

참가 물질

4

반응물 2

HCID 60993N,N-DiethylethylenediamineHCID 214870076,7-dimethoxy-1-phenyl-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride

생성물 1

HCID 21486957HCID 21486957, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 10 parts by volume of 2-diethylaminoethylamine is added 3.0 parts of 6,7-dimethoxy-1-phenyl-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride. An exothermic reaction ensues. The mixture is heated over a steam bath for approximately 30 minutes. (Alternatively, the mixture is maintained at room temperature overnight.) The reaction mixture is then poured into water and extracted with ethyl ether. The ether layer is dried over anhydrous calcium sulfate and evaporated to dryness. The solid thus obtained is crystallized from a mixture of ethyl ether and n-hexane to afford N-(2-diethylaminoethyl)-6,7-dimethoxy-1-phenyl-3,4-dihydro-2(1H)-isoquinolinecarboxamide, melting at about 97°-98°C.

후처리

  1. customAn exothermic reaction
  2. temperatureThe mixture is heated over a steam bath for approximately 30 minutes
  3. extractionextracted with ethyl ether
  4. dry with materialThe ether layer is dried over anhydrous calcium sulfate
  5. customevaporated to dryness
  6. customThe solid thus obtained
  7. customis crystallized from a mixture of ethyl ether and n-hexane

출처 및 근거

ORD 기록
ord-78f928b92249456fb86c9502fac5b461
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001244

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