反応式
[C:1]([NH:4][C:5]1[S:6][CH:7]=[C:8]([CH:10]=[CH:11][C:12]2[S:16][C:15]([C:17]([OH:19])=[O:18])=[CH:14][CH:13]=2)[N:9]=1)(=[O:3])[CH3:2]>O1CCCC1.CO.[C].[Pd]>[C:1]([NH:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][CH2:11][C:12]2[S:16][C:15]([C:17]([OH:19])=[O:18])=[CH:14][CH:13]=2)[N:9]=1)(=[O:3])[CH3:2]参加物
5
実験手順
5-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]vinyl}thiophene-2-carboxylic acid (900.0 mg, 3.058 mmol) was dissolved in a mixed solvent of tetrahydrofuran (250 ml) and methanol (100 ml). 20% Palladium carbon was added, and the mixture was hydrogenated at room temperature under 4 atm. After the completion of the reaction, the reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. Diethyl ether (100 ml) was added to the concentrated residue, and the precipitate was collected by filtration, washed with diethyl ether, and dried under reduced pressure to give 5-{2-[2-(acetylamino)-1,3-thiazol-4-yl]ethyl}thiophene-2-carboxylic acid (738.1 mg, 2.490 mmol, yield 81.4%) as an off-white solid.
後処理
- customwas hydrogenated at room temperature under 4 atm
- customAfter the completion of the reaction
- filtrationthe reaction mixture was filtered through celite
- concentrationthe filtrate was concentrated under reduced pressure
- additionDiethyl ether (100 ml) was added to the concentrated residue
- filtrationthe precipitate was collected by filtration
- washwashed with diethyl ether
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-6c950cf75ba840c38818ccc0ebcef983
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08507690B2
関連ノート
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