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Water → 2-(2,3-Difluorophenyl)-2-methylpropanoic acid

HRID 1868684
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HRID 1868684 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]([CH3:13])([CH3:12])[C:10]#N.[OH2:14].[OH:15]S(O)(=O)=O>O1CCOCC1>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]([CH3:13])([CH3:12])[C:10]([OH:15])=[O:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 11976442HCID 11976442, 화합물

생성물 1

HCID 639898282-(2,3-Difluorophenyl)-2-methylpropanoic acid

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
110 °C

실험 절차

A mixture of 2-(2,3-difluorophenyl)-2-methylpropanenitrile (9.5 g, 52 mmol) in 50 mL dioxane was treated with 10 mL H2O and concentrated H2SO4 (3 mL, 105 mmol). The resulting mixture was stirred at 110° C. for 16 hours, M+1=201. The reaction was then cooled to room temperature. The mixture was extracted with EtOAc and the organic layer discarded. The water layer was acidified with concentrated HCl, extracted with EtOAc, washed with H2O and brine, dried over anhydrous Na2SO4, and concentrated in vacuo to give 4.74 g of the title compound as a pale yellow solid. MS (m/z)=201 (M+H)+.

후처리

  1. temperatureThe reaction was then cooled to room temperature
  2. extractionThe mixture was extracted with EtOAc
  3. extractionextracted with EtOAc
  4. washwashed with H2O and brine
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5fe024172bf442129e5ba8f1084b1dfe
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07635715B2

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