Pyridine → 3,4,5-Trimethoxybenzeneacetyl-1-[(3,4-dimethoxyphenyl)-methylene]isoquinoline

HRID 597242

반응식

HRID 597242 반응식
CO[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1OC)[C:9](=[CH:15][C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([O:24][CH3:25])[CH:17]=1)[NH:8][CH2:7][CH2:6]2.N1C=CC=CC=1.C(N(C(C)C)C(C)C)C.[CH3:41][O:42][C:43]1[CH:44]=[C:45]([CH2:53][C:54](Cl)=[O:55])[CH:46]=[C:47]([O:51][CH3:52])[C:48]=1[O:49][CH3:50]>C(Cl)(Cl)Cl.C1C=CC=CC=1>[CH3:52][O:51][C:47]1[CH:46]=[C:45]([CH2:53][C:54]([C:7]2[NH:8][C:9](=[CH:15][C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([O:24][CH3:25])[CH:17]=3)[C:10]3[C:5]([CH:6]=2)=[CH:4][CH:3]=[CH:12][CH:11]=3)=[O:55])[CH:44]=[C:43]([O:42][CH3:41])[C:48]=1[O:49][CH3:50]

참가 물질

7

반응물 4

HCID 1049PyridineHCID 81531DiisopropylethylamineHCID 110321242-(3,4,5-trimethoxyphenyl)acetyl ChlorideHCID 681233913,4-Dihydro-6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methylene]isoquinoline

생성물 1

HCID 867345733,4,5-Trimethoxybenzeneacetyl-1-[(3,4-dimethoxyphenyl)-methylene]isoquinoline

시약·촉매·용매 2

HCID 241Benzene용매HCID 6212Chloroform용매

실험 절차

To a suspension of 12 parts of 3,4-dihydro-6,7-dimethoxy-1-[(3,4-dimethoxyphenyl)methylene]isoquinoline in 50 parts of pyridine and 5 parts of N-ethyl-N-(1-methylethyl)-2-propanamine is added a solution of 10 parts of 3,4,5-trimethoxybenzeneacetyl chloride in 45 parts of benzene. The resultant mixture is heated at the boiling point under reflux for 1 hour, then cooled and thereupon diluted with 500 parts of chloroform. The resultant solution is washed with water, dried over anhydrous sodium sulfate, and stripped of solvent by vacuum distillation. The residue is crystallized from a mixture of ethyl acetate and ether to give (Z)-1,2,3,4-tetrahydro-6,7-dimethoxy-2-(3,4,5-trimethoxybenzeneacetyl-1-[(3,4-dimethoxyphenyl)-methylene]isoquinoline melting at 164°-170°.

후처리

  1. temperatureunder reflux for 1 hour
  2. temperaturecooled
  3. washThe resultant solution is washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationstripped of solvent by vacuum distillation
  6. customThe residue is crystallized from a mixture of ethyl acetate and ether

출처 및 근거

ORD 기록
ord-9277f6817e6345548df65511f3cdca40
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04013666

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