Carbon Dioxide → Methyl 2,2,3,3-tetrafluoro-3-(methylsulfanyl)propanoate
반응식
C[S-].[Na+].C[S:5]([CH3:7])=O.[F:8][C:9]([F:13])=[C:10]([F:12])[F:11].COS([O:19][CH3:20])(=O)=O.[C:21](=O)=[O:22]>>[CH3:7][S:5][C:9]([C:10]([C:21]([O:19][CH3:20])=[O:22])([F:12])[F:11])([F:13])[F:8]참가 물질
6
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- 온도
- 100 °C
실험 절차
A 400 mL pressure vessel was charged with 34.1 g (0.49 mol) of sodium thiomethoxide and 150 mL of anhydrous dimethylsulfoxide (DMSO). The vessel was closed, cooled in dry ice, evacuated and charged with 32 g (0.73 mol) of carbon dioxide and 50 g (0.5 mol) of tetrafluoroethylene. The vessel contents were heated with agitation to 50° C. for 1 hr and 100° C. for 5 hr. After cooling to room temperature, the vessel contents were transferred to a 500 mL round bottom flask using an additional 30 mL of DMSO to rinse. Dimethylsulfate (65 g, 0.52 mol) was added and the mixture was stirred for 3 hr at 30°-50° C. Volatiles were removed by distillation at 1 mm into a dry ice cooled receiver with a maximum pot temperature of 65° C.
후처리
- customThe vessel was closed
- customevacuated
- temperatureAfter cooling to room temperature
- customthe vessel contents were transferred to a 500 mL round bottom flask
- washto rinse
- customVolatiles were removed by distillation at 1 mm into a dry ice cooled receiver with a maximum pot temperature of 65° C.
출처 및 근거
- ORD 기록
- ord-2c1018bb229d4d8094db72d6bb0fc44b
- 출처 데이터셋
- uspto-grants-1997_09
- 특허 번호
- US05668233
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