Thiophene → HCID 10514014、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=O)=[CH:4][CH:3]=1.[S:12]1[CH:16]=[CH:15][CH:14]=[CH:13]1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([C:13]2[S:12][CH:16]=[CH:15][CH:14]=2)=[O:11])=[CH:6][CH:7]=1参加物
6
実験手順
A mixture of 85.3 g of p-chlorophenylacetic acid and 200 ml of thiophene was stirred at 40° C. as 105 g of trifluoroacetic anhydride was added. The mixture was then refluxed for 4 hrs. It was poured into ice and water and made basic with sodium carbonate. The mixture was extracted with dichloromethane, dried over potassium carbonate and concentrated. The crude yield was 126.4 g. This was recrystallized from 300 ml of methanol to give 103 g, m.p. 98°-99° C.
後処理
- additionwas added
- temperatureThe mixture was then refluxed for 4 hrs
- extractionThe mixture was extracted with dichloromethane
- dry with materialdried over potassium carbonate
- concentrationconcentrated
- customThis was recrystallized from 300 ml of methanol
- customto give 103 g, m.p. 98°-99° C.
出典と根拠
- ORDレコード
- ord-dab0fa3ab1304e4980c4414ac9dd6baa
- 出典データセット
- uspto-grants-1979_06
- 特許番号
- US04159338
反応ノート
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