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Water → 2,4,6-Trifluorobenzyl alcohol

HRID 845502
ノート
印刷プレビュー

反応式

HRID 845502 の反応式
[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]([F:12])[C:3]=1[C:4](O)=[O:5].O>O1CCCC1>[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]([F:12])[C:3]=1[CH2:4][OH:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 962WaterHCID 5203732,4,6-Trifluorobenzoic acid

生成物 1

HCID 27770372,4,6-Trifluorobenzyl alcohol収率 85.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred solution of 4.1 grams (0.023 mole) of 2,4,6-trifluorobenzoic acid in 50 ml of anhydrous tetrahydrofuran, under a nitrogen atmosphere was added dropwise 4.0 grams (0.047 mole) of borane-tetrahydrofuran complex (as 46.6 ml of a 1.0 molar solution in tetrahydrofuran). The addition caused the reaction mixture to foam. Upon completion of addition the reaction mixture was stirred at ambient temperature for two hours, then was heated under reflux for one hour. The reaction mixture was cooled and 50 ml of water was cautiously added. The tetrahydrofuran was removed under reduced pressure and the residue washed into a separatory funnel with 100 ml of aqueous 2N sodium hydroxide. The mixture was extracted with three 100 ml portions of methylene chloride. The combined extracts were dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to give 3.2 grams of 2,4,6-trifluorophenylmethyl alcohol as an oil.

後処理

  1. additionThe addition
  2. additionUpon completion of addition the reaction mixture
  3. temperaturewas heated
  4. temperatureunder reflux for one hour
  5. temperatureThe reaction mixture was cooled
  6. customThe tetrahydrofuran was removed under reduced pressure
  7. washthe residue washed into a separatory funnel with 100 ml of aqueous 2N sodium hydroxide
  8. extractionThe mixture was extracted with three 100 ml portions of methylene chloride
  9. dry with materialThe combined extracts were dried with magnesium sulfate
  10. filtrationfiltered
  11. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-39d88c4fc7b14798adfa52d0ba5bafd2
出典データセット
uspto-grants-1988_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04758590

反応ノート

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