N,N-Diethylethylenediamine → HCID 21486957、化合物

HRID 1414278ノート

反応式

HRID 1414278 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 21486957HCID 21486957、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-78f928b92249456fb86c9502fac5b461
出典データセット
uspto-grants-1977_01
特許番号
US04001244

反応ノート

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