反応式
[I:1][C:2]1[C:6]([CH:7]=O)=[CH:5][N:4]([CH2:9][O:10][CH3:11])[N:3]=1.[F:12][C:13]([F:25])([F:24])[C:14]1[CH:19]=[CH:18][C:17]([S:20]([NH2:23])(=[O:22])=[O:21])=[CH:16][CH:15]=1>C1COCC1.[Cl-].[Na+].O.[O-]CC.[Ti+4].[O-]CC.[O-]CC.[O-]CC>[I:1][C:2]1[C:6]([CH:7]=[N:23][S:20]([C:17]2[CH:16]=[CH:15][C:14]([C:13]([F:12])([F:25])[F:24])=[CH:19][CH:18]=2)(=[O:21])=[O:22])=[CH:5][N:4]([CH2:9][O:10][CH3:11])[N:3]=1参加物
6
反応物 2
生成物 1
試薬・触媒・溶媒 3
実験手順
3-Iodo-1-(methoxymethyl)-1H-pyrazole-4-carbaldehyde (39) (2.0 g, 7.52 mmol) and 4-(trifluoromethyl)benzenesulfonamide (40) (1.69 g, 7.52 mmol) were dissolved in THF (20 mL) under nitrogen. Titanium(IV) ethoxide (7.8 mL, 37.6 mmol) was added via syringe and the reaction stirred for 16 hr at rt. The reaction was poured into brine (50 mL) and filtered through a pad of Celite. The filtrate was extracted with EtOAc (3×50 mL) and the combined organics were washed with brine (100 mL), dried over Na2SO4, and concentrated in vacuo to give N-((3-iodo-1-(methoxymethyl)-1H-pyrazol-4-yl)methylene)-4-(trifluoromethyl)benzenesulfonamide (41) as a clear oil that was used without further purification.
後処理
- filtrationfiltered through a pad of Celite
- extractionThe filtrate was extracted with EtOAc (3×50 mL)
- washthe combined organics were washed with brine (100 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-18b12a13eaee4612ab3c910786c31e50
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07977368B2
関連ノート
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