반응식
[F:1][C:2]([F:10])([F:9])[C:3]([C:5]([F:8])([F:7])[F:6])=[CH2:4].[CH:11]1C[CH:14]=[CH:13][CH:12]=1.[OH:16]O.[CH:18]([OH:20])=O>>[OH:16][CH:11]1[CH:18]([OH:20])[CH:14]2[CH2:13][CH:12]1[CH2:4][C:3]2([C:5]([F:8])([F:7])[F:6])[C:2]([F:10])([F:9])[F:1]참가 물질
반응 조건
- 온도
- 50 °C
실험 절차
5.2 g (20 mmol) of the Diels-Alder reaction product of 3,3,3-trifluoro-2-trifluoromethyl-1-propene (hexafluoroisobutene) and cyclopentadiene are mixed with 20 ml of formic acid, and 1.3 ml of 70 percent strength hydrogen peroxide (30 mmol) is added at 50° C., and the mixture is held at 50° C. for 20 hours. Testing for oxidant using KI-starch paper showed that the oxidant had been broken down completely. The low-boiling components are distilled off under reduced pressure. The residue is heated to 50° C. with 200 ml of 20% strength aqueous sodium hydroxide. The precipitated solid is extracted with a total of 130 ml of methylene chloride. The combined extracts are dried with magnesium sulfate, the methylene chloride is distilled off, and the residue is sublimated at 60° C. in an oil pump vacuum.
후처리
- additionis added at 50° C.
- distillationThe low-boiling components are distilled off under reduced pressure
- extractionThe precipitated solid is extracted with a total of 130 ml of methylene chloride
- dry with materialThe combined extracts are dried with magnesium sulfate
- distillationthe methylene chloride is distilled off
- customis sublimated at 60° C. in an oil pump vacuum
출처 및 근거
- ORD 기록
- ord-af7162bf56cb43e9a873c7fd7f725eb5
- 출처 데이터셋
- uspto-grants-1994_03
- 특허 번호
- US05292971
연결된 노트
불러오는 중…