Benzene → alpha,alpha,alpha,alpha',alpha',alpha'-Hexafluoro-2,4-xylylphenyl ether

HRID 616870

반응식

HRID 616870 반응식
[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]

참가 물질

6

반응물 4

HCID 241BenzeneHCID 8058HexaneHCID 27732091-chloro-2,4-bis(trifluoromethyl)benzeneHCID 23670670Potassium phenoxide

생성물 1

HCID 23344635alpha,alpha,alpha,alpha',alpha',alpha'-Hexafluoro-2,4-xylylphenyl ether수율 73%

시약·촉매·용매 1

HCID 31347Sulfolane용매

실험 절차

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.

후처리

  1. temperatureThe solution is cooled
  2. washthe solution washed twice with water (1 liter, 500 ml.), twice with 10% sodium carbonate solution (~200 ml
  3. dry with materialeach), and water, dried
  4. filtrationfiltered through activated silica gel (18 25 g.)
  5. customthe solvents removed
  6. distillationthe residue distilled

출처 및 근거

ORD 기록
ord-d3b430b2d4ef49fa8e18a1537eadd196
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04076741

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