3-BroMo-1,1,1,2,2-pentafluoropropane synthesis
- Product Name:3-BroMo-1,1,1,2,2-pentafluoropropane
- CAS Number:422-01-5
- Molecular formula:C3H2BrF5
- Molecular Weight:212.94
893556-35-9
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Yield:-
Reaction Conditions:
with lithium bromide in diethylene glycol dimethyl ether at 35 - 60; for 48 h;
Steps:
1
To a 500 mL 3-necked round-bottom flask equipped with a magnetic stir bar, temperature probe, cold water condenser, and addition funnel was charged diglyme (200 mL). Lithium bromide (75.2 g, 866 mmol) was then added in small portions with temperature rises up to 54 °C observed. Once the temperature had dropped to 35 °C, 2.2.3.3.3-pentafluoropropyl 1,1,2,2,3,3,4,4,4-nonaf uorobutane-l-sulfonate (200.1 g, 440 mmol) was added via the addition funnel at a rate which avoided exceeding 40 °C reaction temperature. After complete addition, the resultant reaction mixture was heated to 60 °C followed by a 2 d stir. The reaction mixture was then cooled to room temperature with stirring followed by the addition of water (200 mL). The fluorous layer was collected and washed again with water (2x100 mL) to give the desired 3-bromo-l,l,l,2,2-pentafluoro- propane (75.5 g, 75 mass%, 60% yield). The isolated material was used without further purification for the next step.
References:
WO2020/128964,2020,A2 Location in patent:Page/Page column 18-19
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