1,2-Ethanediamine, N1,N1-bis(1-methylethyl)- → N-(2-diisopropylaminoethyl)-6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarboxamide

HRID 1414283

반응식

HRID 1414283 반응식
[CH:1]([N:4]([CH:8]([CH3:10])[CH3:9])[CH2:5][CH2:6][NH2:7])([CH3:3])[CH3:2].[CH3:11][O:12][C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][C:22]=1[O:23][CH3:24])[CH:19]([C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=1)[N:18]([C:35](Cl)=[O:36])[CH2:17][CH2:16]2.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH:1]([N:4]([CH:8]([CH3:10])[CH3:9])[CH2:5][CH2:6][NH:7][C:35]([N:18]1[CH2:17][CH2:16][C:15]2[C:20](=[CH:21][C:22]([O:23][CH3:24])=[C:13]([O:12][CH3:11])[CH:14]=2)[CH:19]1[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=1)=[O:36])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 84591,2-Ethanediamine, N1,N1-bis(1-methylethyl)-HCID 8471TriethylamineHCID 214869646,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride

생성물 1

HCID 21487010N-(2-diisopropylaminoethyl)-6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarboxamide

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

4.0 Parts of 2-diisopropylaminoethylamine in 75 parts of chloroform is added portionwise, at room temperature, to a mixture of 8.0 parts of 6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarbonyl chloride and 15 parts of triethylamine in 225 parts of chloroform. After the addition is complete, the mixture is stirred for 3 to 4 hours, allowed to stand overnight, and then washed with water. The chloroform layer is separated, dried over anhydrous calcium sulfate and concentrated under reduced pressure. The solid material obtained in this manner is crystallized from ether to give N-(2-diisopropylaminoethyl)-6,7-dimethoxy-1-(3,4-dimethoxyphenyl)-3,4-dihydro-2(1H)-isoquinolinecarboxamide, melting at about 114°-115°C.

후처리

  1. additionAfter the addition
  2. waitto stand overnight
  3. washwashed with water
  4. customThe chloroform layer is separated
  5. dry with materialdried over anhydrous calcium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe solid material obtained in this manner
  8. customis crystallized from ether

출처 및 근거

ORD 기록
ord-3668809edd3f4ec5a21be884fe9ad38e
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001244

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