Thiophene → HCID 10514014, 화합물
반응식
[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]=1참가 물질
6
실험 절차
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.
후처리
- 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.
출처 및 근거
- ORD 기록
- ord-dab0fa3ab1304e4980c4414ac9dd6baa
- 출처 데이터셋
- uspto-grants-1979_06
- 특허 번호
- US04159338
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