Triethylamine → HCID 18172460, 화합물

HRID 397063

반응식

HRID 397063 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 18172460HCID 18172460, 화합물수율 56.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-88f163b020a4417a8afec3291f8f5e4c
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06608203B2

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