反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([CH3:11])=[C:8](I)[CH:9]=1)=[O:4].[F:12][C:13]1[CH:36]=[CH:35][CH:34]=[C:33]([F:37])[C:14]=1[C:15]([NH:17][C:18]1[CH:23]=[CH:22][C:21](B2OC(C)(C)C(C)(C)O2)=[CH:20][CH:19]=1)=[O:16].C(=O)(O)[O-].[Na+].O>[Pd].C1(C)C=CC=CC=1.CCOC(C)=O.C(O)C>[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([CH3:11])=[C:8]([C:21]2[CH:22]=[CH:23][C:18]([NH:17][C:15](=[O:16])[C:14]3[C:13]([F:12])=[CH:36][CH:35]=[CH:34][C:33]=3[F:37])=[CH:19][CH:20]=2)[CH:9]=1)=[O:4]参加物
9
反応物 4
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 100 °C
実験手順
A mixture of 4-Iodo-5-methyl-thiophene-2-carboxylic acid methyl ester (d, 1 mmol), 2,6-Difluoro-N-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-benzamide (c, 1 mmol), palladium catalyst (0.1 mmol), sodium bicarbonate (1 mmol) in a mixture of toluene (5 mL), water (1 mL), ethanol (1 mL) was heated at 100° C. for 24 h. The mixture was taken up with EtOAc (100 mL), washed with water (2×100 mL) and dried (Na2SO4). The oil obtained on concentration was purified by flash chromatography to give 4-[4-(2,6-Difluoro-benzoylamino)-phenyl]-5-methyl-thiophene-2-carboxylic acid methyl ester as a yellowish solid (50 mg).
後処理
- washwashed with water (2×100 mL)
- dry with materialdried (Na2SO4)
- customThe oil obtained on concentration
- customwas purified by flash chromatography
出典と根拠
- ORDレコード
- ord-c137a143d20840a7ba1a1fd853ece3d9
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08435996B2
関連ノート
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