6-Methoxypyridazin-3-amine → HCID 117925948, 화합물

HRID 594130

반응식

HRID 594130 반응식
[CH3:1][O:2][C:3]1[N:8]=[N:7][C:6]([NH2:9])=[CH:5][CH:4]=1.[CH3:10][C:11]1[C:15]([CH2:16][O:17][C:18]2[CH:23]=[CH:22][C:21]([S:24](Cl)(=[O:26])=[O:25])=[CH:20][CH:19]=2)=[C:14]([CH3:28])[O:13][N:12]=1>N1C=CC=CC=1>[CH3:10][C:11]1[C:15]([CH2:16][O:17][C:18]2[CH:19]=[CH:20][C:21]([S:24]([NH:9][C:6]3[N:7]=[N:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)(=[O:26])=[O:25])=[CH:22][CH:23]=2)=[C:14]([CH3:28])[O:13][N:12]=1

참가 물질

4

반응물 2

HCID 816736-Methoxypyridazin-3-amineHCID 164907024-((3,5-Dimethylisoxazol-4-yl)methoxy)benzene-1-sulfonyl chloride

생성물 1

HCID 117925948HCID 117925948, 화합물수율 4.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
20 °C

실험 절차

To a solution of 6-methoxypyridazin-3-amine (125 mg, 1.0 mmol) in pyridine (8 mL) at room temperature, was added 4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}benzenesulfonyl chloride (0.302 g, 1.0 mmol). The reaction mixture was stirred at 20° C. for 18 hours. The solvent was evaporated in vacuo and passed through an aminopropyl (NH2) solid phase extraction (SPE) cartridge eluting with methanol, followed by a sulphonic acid (SCX) SPE cartridge eluting with methanol. The crude was then purified by flash silica (Si) chromatography (0-100% ethyl acetate-cyclohexane+0-25% methanol gradient), to provide the title compound (16 mg). LCMS (2 min, formic) Rt 0.83 min, m/z (ES+) 391 (M+H).

후처리

  1. customThe solvent was evaporated in vacuo
  2. extractionpassed through an aminopropyl (NH2) solid phase extraction (SPE) cartridge
  3. washeluting with methanol
  4. washeluting with methanol
  5. customThe crude was then purified by flash silica (Si) chromatography (0-100% ethyl acetate-cyclohexane+0-25% methanol gradient)

출처 및 근거

ORD 기록
ord-a6f100bcc13f4355b07a0d68d4972464
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242972B2

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