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

HRID 260794

反応式

HRID 260794 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 214662732-Trifluoromethyl-4-(4-ethoxyphenoxy)-1-benzyloxybenzene収率 41.8%

試薬・触媒・溶媒 1

HCID 23978Copper触媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-98cf78ada01347c892953c47b824b79e
出典データセット
uspto-grants-1996_06
特許番号
US05530015

関連ノート

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