Methyl iodide → HCID 68815178, 화합물

HRID 1436607노트

반응식

HRID 1436607 반응식
[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([N:10]([CH3:14])[CH2:11][CH2:12][CH3:13])[N:7]=[C:6]([NH:15][S:16]([CH3:19])(=[O:18])=[O:17])[CH:5]=1.IC.[C:23](=O)([O-])[O-].[K+].[K+]>CN(C=O)C.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([N:10]([CH3:14])[CH2:11][CH2:12][CH3:13])[N:7]=[C:6]([N:15]([S:16]([CH3:19])(=[O:18])=[O:17])[CH3:23])[CH:5]=1

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 68814746HCID 68814746, 화합물

생성물 1

HCID 68815178HCID 68815178, 화합물

시약·촉매·용매 3

HCID 74236Tetrabutylammonium Bromide촉매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Dissolve 2-methanesulfonylamino-6-(methylpropylamino)-isonicotinic acid methyl ester (87 mg, 2.89 mmol) and iodomethane (0.27 mL, 4.33 mmoles) in DMF (10 mL). Add potassium carbonate (639 mg, 4.62 mmol) and tetrabutylammonium bromide (93 mg, 0.98 mmol) and stir at room temperature 1 h. Dilute with ethyl acetate (80 mL), wash with 10% aqueous potassium carbonate (2×15 mL), 0.1 N citric acid (2×15 mL), 1 N lithium chloride (2×15 mL) and saturated aqueous sodium chloride (15 mL).

후처리

  1. washwash with 10% aqueous potassium carbonate (2×15 mL), 0.1 N citric acid (2×15 mL), 1 N lithium chloride (2×15 mL) and saturated aqueous sodium chloride (15 mL)

출처 및 근거

ORD 기록
ord-f24233d4099447f5919bf0db02c51264
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618978B2

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