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Water → alpha-Methoxy-beta-[4-(4-trifluoromethylphenoxy)phenoxy]propane

HRID 2419158
ノート
印刷プレビュー

反応式

HRID 2419158 の反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:18]=[CH:17][C:11]([O:12][CH:13]([CH3:16])[CH2:14][OH:15])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.[Na].[CH3:24]I.O>O1CCOCC1>[CH3:24][O:15][CH2:14][CH:13]([O:12][C:11]1[CH:17]=[CH:18][C:8]([O:7][C:6]2[CH:19]=[CH:20][C:3]([C:2]([F:21])([F:22])[F:1])=[CH:4][CH:5]=2)=[CH:9][CH:10]=1)[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 5360545SodiumHCID 128048852-{4-[4-(Trifluoromethyl)phenoxy]phenoxy}propan-1-ol

生成物 1

HCID 23332249alpha-Methoxy-beta-[4-(4-trifluoromethylphenoxy)phenoxy]propane収率 67%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane
溶媒

実験手順

6 g of β-[4-(4-trifluoromethylphenoxy)phenoxy]propanol was dissolved in 30 ml of dioxane and 0.46 g of sodium was added to the solution. The mixture was then heated for 3 hours while refluxing. 3.1 g of methyl iodide was added thereto and the resulting mixture was heated for 6 hours while refluxing. The reaction mixture was then poured into an appropriate amount of water and extracted with diethyl ether. The extract was washed with water and dried over anhydrous sodium sulfate. The ether was removed by distillation and the residue was distilled under reduced pressure to obtain 4.2 g of the desired product having a boiling point of 160° to 165° C/2 mmHg.

後処理

  1. temperatureThe mixture was then heated for 3 hours
  2. temperaturewhile refluxing
  3. temperaturethe resulting mixture was heated for 6 hours
  4. temperaturewhile refluxing
  5. extractionextracted with diethyl ether
  6. washThe extract was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe ether was removed by distillation
  9. distillationthe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-5ac17d9642054ae297491504eae5d148
出典データセット
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04105435

反応ノート

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