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Water → Ethyl difluoro(3,4,5-trifluorophenoxy)acetate

HRID 1399417
ノート
印刷プレビュー

反応式

HRID 1399417 の反応式
C(=O)([O-])[O-].[K+].[K+].[F:7][C:8]1[CH:9]=[C:10]([OH:16])[CH:11]=[C:12]([F:15])[C:13]=1[F:14].Br[C:18]([F:25])([F:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20].O>CCCC[N+](CCCC)(CCCC)CCCC.[Br-].CN(C=O)C>[F:7][C:8]1[CH:9]=[C:10]([CH:11]=[C:12]([F:15])[C:13]=1[F:14])[O:16][C:18]([F:25])([F:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 69585Ethyl bromodifluoroacetateHCID 27779433,4,5-Trifluorophenol

生成物 1

HCID 21057440Ethyl difluoro(3,4,5-trifluorophenoxy)acetate収率 69.4%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide
触媒
HCID 6228Dimethylformamide溶媒2 回

実験手順

Under a nitrogen atmosphere, 17 g of potassium carbonate and 4.0 g of TBAB were added to 18 g of 3,4,5-trifluorophenol (r-7) dissolved in 200 mL of DMF, 25.0 g of ethyl bromodifluoroacetate dissolved in 50 mL of DMF was added thereto, and the resultant mixture was stirred at 90° C. for 3 hours. A reaction mixture was poured into water, subjected to extraction with diethyl ether, and extracted organic layers were combined and washed with saturated brine, and then dried over anhydrous magnesium sulfate. A solvent was evaporated under reduced pressure, and thus 22.8 g of ethyl 2-(3,4,5-trifluorophenoxy)-2,2-difluoroacetate (compound (r-8)) was obtained.

後処理

  1. additionwas added
  2. extractionsubjected to extraction with diethyl ether
  3. extractionextracted organic layers
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customA solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-5dd0b2eeefca409d8c1d31b7a20ad022
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08906260B2

反応ノート

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