Reaction equation
[O-:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[K+].Cl[C:10]1[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][C:11]=1[C:20]([F:23])([F:22])[F:21].[CH:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[CH3:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35]>S1(CCCC1)(=O)=O>[F:21][C:20]([F:23])([F:22])[C:11]1[CH:12]=[C:13]([C:16]([F:19])([F:18])[F:17])[CH:14]=[CH:15][C:10]=1[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[O:1][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[C:32]1[CH:31]=[CH:30][C:35]([C:16]([F:19])([F:18])[F:17])=[CH:34][C:33]=1[C:20]([F:23])([F:22])[F:21]Participants
6
Procedure
A solution of potassium phenoxide (15.0 g. 0.1 m) and 4-chloro-α,α,α,α',α',α'-hexafluoro-m-xylene in sulfolane (50 ml.) is heated 60 hours at 140°-160° C. The solution is cooled and benzene (400 ml.) and hexane (250 ml.) are added and the solution washed twice with water (1 liter, 500 ml.), twice with 10% sodium carbonate solution (~200 ml. each), and water, dried, filtered through activated silica gel (18 25 g.), the solvents removed, and the residue distilled to give α,α,α,α',α',α'-hexafluoro-2,4-xylylphenyl ether (22.4 g., 73%) b.p. 81°-85° C./~1 mm.
Workup
- temperatureThe solution is cooled
- washthe solution washed twice with water (1 liter, 500 ml.), twice with 10% sodium carbonate solution (~200 ml
- dry with materialeach), and water, dried
- filtrationfiltered through activated silica gel (18 25 g.)
- customthe solvents removed
- distillationthe residue distilled
Sources & evidence
- ORD record
- ord-7aaeb38891b445e2967c66a32cae9096
- Source dataset
- uspto-grants-1980_08
- Patent number
- USRE030361
Linked notes
Loading…