Hydrochloric Acid → 2-Trifluoromethyl-4-(4-ethoxyphenoxy)-1-benzyloxybenzene

HRID 260794

반응식

HRID 260794 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:4]([C:16]([F:19])([F:18])[F:17])[CH:3]=1.[CH2:20]([O:22][C:23]1[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=1)[CH3:21].C(=O)([O-])[O-].[K+].[K+].Cl>[Cu]>[F:17][C:16]([F:19])([F:18])[C:4]1[CH:3]=[C:2]([O:29][C:26]2[CH:27]=[CH:28][C:23]([O:22][CH2:20][CH3:21])=[CH:24][CH:25]=2)[CH:7]=[CH:6][C:5]=1[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 121504-EthoxyphenolHCID 186201601-(Benzyloxy)-4-bromo-2-(trifluoromethyl)benzene

생성물 1

HCID 214662732-Trifluoromethyl-4-(4-ethoxyphenoxy)-1-benzyloxybenzene수율 41.8%

시약·촉매·용매 1

HCID 23978Copper촉매

실험 절차

Then, 5.10 g of 4-bromo-2-trifluoromethyl-1-benzyloxybenzene, 2.34 g of p-ethoxyphenol, 2.13 g of potassium carbonate, 100 mg of copper and 200 mg of cuprous chloride were charged into a reaction vessel, and stirred at 130° C. to 140° C. for 5 hours. The reaction solution was cooled to room temperature, poured into ice-water and then acidified by adding 10% hydrochloric acid. The solution was extracted twice with 100 ml of diethyl ether. Then, the ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 2.50 g of 2-trifluoromethyl-4-(4-ethoxyphenoxy)-1-benzyloxybenzene (yield, 41%).

후처리

  1. extractionThe solution was extracted twice with 100 ml of diethyl ether
  2. washwashed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customto give a crude product

출처 및 근거

ORD 기록
ord-98cf78ada01347c892953c47b824b79e
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530015

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