Sodium Hydroxide → HCID 13851426、化合物
反応式
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[S:10][CH2:11][CH2:12][C:13]([OH:15])=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[CH3:9][O:8][C:6]1[CH:7]=[C:2]([CH3:1])[C:3]2[S:10][CH2:11][CH2:12][C:13](=[O:15])[C:4]=2[CH:5]=1参加物
4
実験手順
A solution of 21.1 g 3-[(2-methyl-4-methoxyphenyl)thio]propanoic acid and 160 g polyphosphoric ester in 150 ml CHCl3 is refluxed for 45 min. To the cooled reaction mixture is added 200 ml 0.5 N NaOH. The organic phase is separated and the aqueous phase is extracted with 100 ml CHCl3. The combined organic extracts are dried over Na2SO4, filtered, concentrated under reduced pressure and flash chromatrographed with ethyl acetate/hexane (8:92) to yield 6-methoxy-8-methyl-2H-[1]benzothiopyran-4-one.
後処理
- customTo the cooled reaction mixture
- customThe organic phase is separated
- extractionthe aqueous phase is extracted with 100 ml CHCl3
- dry with materialThe combined organic extracts are dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure and flash
出典と根拠
- ORDレコード
- ord-61e2149a19f14ec29612012cdcb98da1
- 出典データセット
- uspto-grants-1987_05
- 特許番号
- US04666916
反応ノート
読み込み中…