Methanol → Methyl 3-phenylmethylthiopyridine-4-carboxylate
反応式
[C:1]1([CH2:7][C:8]2[CH:9]=[N:10][CH:11]=[CH:12][C:13]=2[C:14]([OH:16])=[S:15])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.[CH3:22]O>COC(OC)(C)C>[C:1]1([CH2:7][C:8]2[CH:9]=[N:10][CH:11]=[CH:12][C:13]=2[C:14]([O:16][CH3:22])=[S:15])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1参加物
5
実験手順
A solution of 5.1 g (20 mmol) of 3-phenylmethylthiopyridine-4-carboxylic acid in 150 mL of methanol, 1.6 mL of 2,2-dimethoxypropane, and 5 mL of sulfuric acid was heated at reflux for 18 hours. The solution was cooled, concentrated to 25 mL, then partitioned between ether and sodium bicarbonate solution. The ether layer was washed with sodium bicarbonate solution, then brine, then dried and concentrated to afford 5.0 g (96%) of white crystals, m.p. 79°-80° C.
後処理
- temperatureat reflux for 18 hours
- temperatureThe solution was cooled
- concentrationconcentrated to 25 mL
- custompartitioned between ether and sodium bicarbonate solution
- washThe ether layer was washed with sodium bicarbonate solution
- dry with materialbrine, then dried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9626ea8265e140e9919731623ca102ec
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04767766
反応ノート
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