6,7-Dimethoxy-1,2,3,4-Tetrahydroisoquinoline → HCID 178418719、化合物

HRID 8713

反応式

HRID 8713 の反応式
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

参加物

4

反応物 2

HCID 156236,7-Dimethoxy-1,2,3,4-TetrahydroisoquinolineHCID 178418955HCID 178418955、化合物

生成物 1

HCID 178418719HCID 178418719、化合物収率 50.3%

試薬・触媒・溶媒 1

HCID 30156371-Methoxyethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3ea103740d49442d947174854bfe2809
出典データセット
uspto-grants-2006_08
特許番号
US07091200B2

関連ノート

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