Potassium Hydroxide → 2-(2,4-Difluorophenyl)-1,2,3-propanetriol

HRID 1003775

反応式

HRID 1003775 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:20])([CH2:15][O:16]C(=O)C)[CH2:10][O:11]C(=O)C.[OH-].[K+]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:20])([CH2:15][OH:16])[CH2:10][OH:11]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 154634621,3-Diacetoxy-2-(2,4-difluorophenyl)-2-propanol

生成物 1

HCID 112179522-(2,4-Difluorophenyl)-1,2,3-propanetriol収率 91.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

In a 200 ml reaction vessel, 10 g of 2-(2,4-difluorophenyl)-1,3-diacetoxy-2-propanol was dissolved in 30 ml of toluene and thereto was added 30 ml of 30% aqueous KOH solution. The resulting liquid was stirred at room temperature for 24 hours and more. Then a toluene-layer and an aqueous layer were separated from each other and the aqueous layer was extracted twice with 50 ml of ethyl acetate. The organic layer was washed with brine and then dried over anhydrous sodium sulfate. The solvent was removed therefrom and the residue was purified in the same manner as in Example 32 to give 6.5 g of 2-(2,4-difluorophenyl)-1,2,3-propanetriol.

後処理

  1. customThen a toluene-layer and an aqueous layer were separated from each other and the aqueous layer
  2. extractionwas extracted twice with 50 ml of ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed
  6. customthe residue was purified in the same manner as in Example 32

出典と根拠

ORDレコード
ord-90629b655faa4ab5b122bbc9f95bfe3f
出典データセット
uspto-grants-2000_04
特許番号
US06046354

関連ノート

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