Sodium Hydroxide → 1,2-Difluoro-4,5-dimethylbenzene
Reaction equation
Cl[C:2]1([F:12])[CH2:7][C:6]([CH3:8])=[C:5]([CH3:9])[CH2:4][C:3]1(F)[F:10].[OH-].[Na+]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[F:10][C:3]1[CH:4]=[C:5]([CH3:9])[C:6]([CH3:8])=[CH:7][C:2]=1[F:12]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
To a stirred solution of 5-chloro-1,2-dimethyl-4,4,5-trifluorocyclohexene of 12.6 g prepared in Example 14 was added 1.0 g of benzyltriethylammonium chloride, and then the reaction mixture was heated to 80° C. followed by slowly adding 40 g of 50% aqueous sodium hydroxide solution for 30 min. The reaction mixture was stirred for additional 2 hours at 80° C., and then the resultant was purified by steam distillation followed by separating the aqueous layer. The organic layer was dried with calcium chloride, and then 7.3 g of the desired product was collected by fractional distillation at temperature 150° C. as a colorless liquid.
Workup
- distillationthe resultant was purified by steam distillation
- customby separating the aqueous layer
- dry with materialThe organic layer was dried with calcium chloride
- distillation7.3 g of the desired product was collected by fractional distillation at temperature 150° C. as a colorless liquid
Sources & evidence
- ORD record
- ord-d168ffdbc1464913baf518db1544ccdc
- Source dataset
- uspto-grants-1999_12
- Patent number
- US06008407
Reaction notes
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