反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6](=[O:10])[C:7]([OH:9])=O.C(Cl)(=O)C(Cl)=O.[CH3:17][N:18]([CH3:25])[CH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.CCN(C(C)C)C(C)C>C(Cl)Cl.CN(C)C1C=CN=CC=1.CN(C=O)C>[CH3:17][N:18]([CH3:25])[CH:19]1[CH2:24][CH2:23][N:22]([C:7](=[O:9])[C:6]([C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)=[O:10])[CH2:21][CH2:20]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 3
実験手順
2-Thiopheneglyoxylic acid (300 mg, 1.9 mmol) was dissolved in 10 mL of methylene chloride. A 2.0 M solution of oxalyl chloride in methylene chloride (1.1 mL, 2.1 mmol) was then added, followed by 10 μL of DMF. The resulting solution was stirred at room temperature for 1 hour, then a solution of dimethylpiperidin-4-ylamine (271 mg, 2.1 mmol) and DIPEA (1.0 mL, 5.8 mmol) in 2 mL of methylene chloride was added. 4-Dimethylaminopyridine (12 mg, 96 μmol) was then added and the resulting mixture was stirred at room temperature for 2 hours. The mixture was then extracted with a saturated sodium bicarbonate solution, and the organic layer was dried over Na2SO4 and concentrated to yield the crude intermediate (4a) (498 mg), which was used in the next step without further purification.
後処理
- stirringthe resulting mixture was stirred at room temperature for 2 hours
- extractionThe mixture was then extracted with a saturated sodium bicarbonate solution
- dry with materialthe organic layer was dried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-41b1e7b8df8c44c797c03d084b8e46d5
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08202891B2
関連ノート
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