Hydrogen Peroxide → HCID 19097010, compound
Reaction equation
[F:1][C:2]([F:9])([F:8])[C:3]([F:7])=[C:4]([F:6])[F:5].[CH:10]1[CH2:14][CH:13]=[CH:12][CH:11]=1.S(=O)(=O)(O)[OH:16].OO.[OH2:22]>>[OH:22][CH:11]1[CH:10]([OH:16])[CH:14]2[CH2:13][CH:12]1[C:4]([F:6])([F:5])[C:3]2([F:7])[C:2]([F:9])([F:8])[F:1]Participants
6
Conditions
- Temperature
- 60 °C
Procedure
4.3 g (20 mmol) of the Diels-Alder reaction product of hexafluoropropene and cyclopentadiene are mixed with 10 ml of water, 1 ml of 30 percent strength sulfuric acid and 400 mg of the catalyst [CH3N(C8H17)3 ][PO4 {W(O)(O2)2 }4 ]whose preparation is described in Synthesis 296 (1989), and the mixture is heated to 60° C. 1.7 ml (40 mmol) of 70 percent strength hydrogen peroxide is then added, and the emulsion is kept at 60° C. for 6 hours. Upon cooling, a white solid precipitates which is filtered off with suction and washed with cold water. The crude product is then purified by sublimation at a pressure of 0.1 mbar and a temperature of 50 ° C.
Workup
- customis described in Synthesis 296 (1989)
- temperatureUpon cooling
- customa white solid precipitates which
- filtrationis filtered off with suction
- washwashed with cold water
- customThe crude product is then purified by sublimation at a pressure of 0.1 mbar
- customa temperature of 50 ° C.
Sources & evidence
- ORD record
- ord-57bc493b21284ceca52f040ac9101d5b
- Source dataset
- uspto-grants-1994_03
- Patent number
- US05292971
Reaction notes
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