Triethylamine → HCID 18172460、化合物

HRID 397063

反応式

HRID 397063 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([CH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)=[N:8][CH2:7][CH2:6]2.C(N(CC)CC)C.[CH3:26][N:27]1[CH:31]=[C:30]([S:32](Cl)(=[O:34])=[O:33])[N:29]=[CH:28]1>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([CH:13]1[CH2:18][CH2:17][N:16]([S:32]([C:30]3[N:29]=[CH:28][N:27]([CH3:26])[CH:31]=3)(=[O:34])=[O:33])[CH2:15][CH2:14]1)=[N:8][CH2:7][CH2:6]2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27368871-methyl-1H-imidazole-4-sulfonyl chlorideHCID 181723896-Methoxy-1-piperidin-4-yl-3,4-dihydro-isoquinoline

生成物 1

HCID 18172460HCID 18172460、化合物収率 56.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred solution of 6-methoxy-1-piperidin-4-yl-3,4-dihydro-isoquinoline (0.094 g, 0.385 mmol) and triethylamine (0.078 g, 0.77 mmol) in CH2Cl2 (3 ml) was added 1-methyl-1H-imidazole-4-sulfonyl chloride (0.070 g, 0.385 mmol). The reaction mixture was stirred at RT under an atmosphere of N2 overnight. The reaction mixture was diluted with CH2Cl2 (10 ml) and washed with water (2×5 ml). The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified via radial chromatography (SiO2, 1 mm, CH2Cl2 to 5% MeOH/CH2Cl2) to give the product as an oil (0.084 g, 0.216 mmol, 56% yield).

後処理

  1. washwashed with water (2×5 ml)
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified via radial chromatography (SiO2, 1 mm, CH2Cl2 to 5% MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-88f163b020a4417a8afec3291f8f5e4c
出典データセット
uspto-grants-2003_08
特許番号
US06608203B2

関連ノート

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