Methanol → HCID 12021304、化合物
反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([CH2:11][C:12]([OH:14])=[O:13])[CH:9]=2)[CH:4]=[CH:3][CH:2]=1.O=S(Cl)Cl.[CH3:19]O>CN(C)C=O>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([CH2:11][C:12]([O:14][CH3:19])=[O:13])[CH:9]=2)[CH:4]=[CH:3][CH:2]=1参加物
5
実験手順
To a solution of example 11A (1.98 g, 10.59 mmol) in 40 mL of anhydrous methanol was slowly added SOCl2 (1.5 mL, 31.7 mmol), and a drop of dimethylformamide as catalyst. The mixture was refluxed for 5 hrs and then concentrated under reduced pressure. The residue was dissolved in water (10 mL) and neutralized with aqueous sodium bicarbonate to pH 8. The product was extracted with methylene chloride, dried with anhydrous sodium sulfate and concentrated under reduced pressure to afford 2.13 g of the title compound. MS (ESI+) m/z 202 (M+H)+.
後処理
- temperatureThe mixture was refluxed for 5 hrs
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in water (10 mL)
- extractionThe product was extracted with methylene chloride
- dry with materialdried with anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-27995b58fe0d42b6ae981bb298cddc14
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07241776B2
反応ノート
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