Sodium Hydroxide → HCID 23291416、化合物
反応式
C[O:2][C:3]([C:5]1[CH:6]=[CH:7][CH:8]=[C:9]2[C:14]=1[S:13][CH2:12][CH2:11][CH2:10]2)=[O:4].[OH-].[Na+]>C(O)C>[S:13]1[C:14]2[C:9](=[CH:8][CH:7]=[CH:6][C:5]=2[C:3]([OH:4])=[O:2])[CH2:10][CH2:11][CH2:12]1参加物
4
実験手順
Methylthiochroman-8-carboxylate (0.220 g, 1.05 mmol) was dissolved in ethanol (5 ml) and treated with 10% sodium hydroxide solution (10 ml). The mixture was then heated to reflux with stirring. After 5 h, the reaction mixture was allowed to cool. The ethanol present was then removed by evaporation under reduced pressure. The aqueous residue was then washed with CH2Cl2 (2×) before being acidified to pH1 using 5M HCl. The resultant pale yellow precipitate was then filtered off and dried in vacuo to give the title compound (0.156 g, 76%) (D6).
後処理
- temperatureThe mixture was then heated
- temperatureto reflux
- temperatureto cool
- customThe ethanol present was then removed by evaporation under reduced pressure
- washThe aqueous residue was then washed with CH2Cl2 (2×)
- filtrationThe resultant pale yellow precipitate was then filtered off
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-4edbe41fac814bf4b581065929cd5786
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06127379
反応ノート
読み込み中…