反応式
[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([NH:18][C:19]3[C:24]([CH3:25])=[CH:23][C:22]([CH3:26])=[CH:21][N:20]=3)(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:27])[O:4][N:3]=1.[CH3:28][C:29](N=C(N(C)C)N(C)C)([CH3:31])[CH3:30].BrCC(C)C>C(#N)C>[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([N:18]([C:19]3[C:24]([CH3:25])=[CH:23][C:22]([CH3:26])=[CH:21][N:20]=3)[CH2:28][CH:29]([CH3:31])[CH3:30])(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:27])[O:4][N:3]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}-N-(3,5-dimethyl-2-pyridinyl)benzenesulfonamide (56 mg, 0.145 mmol) in acetonitrile (1 mL) was added N″-(1,1-dimethylethyl)-N,N,N′,N′-tetramethylguanidine (25 mg, 0.145 mmol) and the mixture was stirred at room temperature for 1 hour, 1-bromo-2-methylpropane (0.031 mL, 0.289 mmol) was then added and the mixture was stirred at 70° C. for 125 hours. The mixture was concentrated in vacuo and partitioned between dichloromethane (5 mL) and water (5 mL). The organic layer was then purified by mass directed autoprep (formic acid modifier) to give the title compound (30 mg) as a white solid. LCMS (2 min, formic) Rt 1.31 min, m/z (ES+) 444 (M+H).
後処理
- stirringthe mixture was stirred at 70° C. for 125 hours
- concentrationThe mixture was concentrated in vacuo
- custompartitioned between dichloromethane (5 mL) and water (5 mL)
- customThe organic layer was then purified by mass
出典と根拠
- ORDレコード
- ord-c2bc17e51b0d4e6f8d5cbd9ffc9d4aa7
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09242972B2
関連ノート
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