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[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][N:20]=3)(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:26])[O:4][N:3]=1.[C:27](N=C(N(C)C)N(C)C)([CH3:30])([CH3:29])[CH3:28].BrCC(C)C>C(#N)C>[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([N:18]([CH2:28][CH:27]([CH3:30])[CH3:29])[C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][N:20]=3)(=[O:17])=[O:16])=[CH:13][CH:14]=2)=[C:5]([CH3:26])[O:4][N:3]=1参加物
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-dimethylisoxazol-4-yl)methoxy)-N-(5-methylpyridin-2-yl)benzenesulfonamide (187 mg, 0.5 mmol) in acetonitrile (5 mL) stirred at room temperature, was added 2-(tert-butyl)-1,1,3,3-tetramethylguanidine (0.261 mL, 1.250 mmol). The mixture was stirred at room temperature for 1 hour, then 1-bromo-2-methylpropane (0.190 mL, 1.750 mmol) added. The reaction was then heated by microwaves to 160° C., for 25 minutes. After cooling, dicholormethane (5 mL) was added to the mixture and the organic phase washed with water (5 mL) then separated using a hydrophobic frit. The solvent was removed under a stream of nitrogen and the crude sample purified by mass directed autoprep (ammonium carbonate modifier) to give the title product (8.5 mg). LCMS (3 min, High pH) Rt 1.88 min, m/z (ES+) 430 (M+H).
後処理
- temperatureThe reaction was then heated by microwaves to 160° C., for 25 minutes
- temperatureAfter cooling
- additiondicholormethane (5 mL) was added to the mixture
- washthe organic phase washed with water (5 mL)
- customthen separated
- customThe solvent was removed under a stream of nitrogen
- customthe crude sample purified by mass
出典と根拠
- ORDレコード
- ord-84ca2019465b432baac42525ba1c3256
- 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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