Nitromethane → 1,1-Difluoro-3-nitropropan-2-ol
Reaction equation
C([O:3][CH:4](O)[CH:5]([F:7])[F:6])C.[CH3:9][N+:10]([O-:12])=[O:11].C([O-])([O-])=O.[Na+].[Na+]>O>[F:6][CH:5]([F:7])[CH:4]([OH:3])[CH2:9][N+:10]([O-:12])=[O:11]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 60 °C
Procedure
A mixture of 1-ethoxy-2,2-difluoroethanol (60 g, 0.47 mol), CH3NO2 (32.9 g, 0.56 mol) and Na2CO3 (3 g) was stirred at 60° C. for 3 hrs, then at rt overnight. The mixture was diluted with water (40 mL), extracted with tert-butyl methyl ether (200 mL) and the organic layer was dried over Na2SO4 and concentrated under low temperature to give the title compound, which was used for next step directly.
Workup
- customat rt
- customovernight
- extractionextracted with tert-butyl methyl ether (200 mL)
- dry with materialthe organic layer was dried over Na2SO4
- concentrationconcentrated under low temperature
Sources & evidence
- ORD record
- ord-2a586c71616246b7b1162449013a2b47
- Source dataset
- uspto-grants-2015_05
- Patent number
- US09040547B2
Reaction notes
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