6,7-Dimethoxy-1,2,3,4-Tetrahydroisoquinoline → HCID 178418719, 화합물

HRID 8713

반응식

HRID 8713 반응식
Cl[C:2]1[NH:3][S:4](=[O:17])(=[O:16])[C:5]2[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:6]=2[N:7]=1.[CH3:18][O:19][C:20]1[CH:21]=[C:22]2[C:27](=[CH:28][C:29]=1[O:30][CH3:31])[CH2:26][NH:25][CH2:24][CH2:23]2>COC(O)C>[CH3:18][O:19][C:20]1[CH:21]=[C:22]2[C:27](=[CH:28][C:29]=1[O:30][CH3:31])[CH2:26][N:25]([C:2]1[NH:3][S:4](=[O:17])(=[O:16])[C:5]3[CH:11]=[C:10]([O:12][CH3:13])[C:9]([O:14][CH3:15])=[CH:8][C:6]=3[N:7]=1)[CH2:24][CH2:23]2

참가 물질

4

반응물 2

HCID 156236,7-Dimethoxy-1,2,3,4-TetrahydroisoquinolineHCID 178418955HCID 178418955, 화합물

생성물 1

HCID 178418719HCID 178418719, 화합물수율 50.3%

시약·촉매·용매 1

HCID 30156371-Methoxyethanol용매

실험 절차

3-Chloro-6,7-dimethoxy-2H-benzo[1,2,4]thiadiazine-1,1-dioxide 1a (154 mg, 0.55 mmol) and 6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline 2a (wherein R1 and R4 are hydrogen, and R2 and R3 are methoxy) (138 mg, 0.6 mmol) were dissolved in 20 ml of methoxyethanol and heated at reflux for 72 h. The solvent was removed under reduced pressure. The gummy residue was triturated with isopropanol and the resulting crystals filtered. Recrystallization from dichloromethane afforded 120 mg of 3-(6,7-dimethoxy-3,4-dihydro-1H-isoquinolin-2-yl)-6,7-dimethoxy-2H-benzo[1,2,4]thiadiazine-1,1-dioxide 101, [M+H]+=434.

후처리

  1. temperatureheated
  2. temperatureat reflux for 72 h
  3. customThe solvent was removed under reduced pressure
  4. customThe gummy residue was triturated with isopropanol
  5. filtrationthe resulting crystals filtered
  6. customRecrystallization from dichloromethane

출처 및 근거

ORD 기록
ord-3ea103740d49442d947174854bfe2809
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091200B2

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