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Potassium Carbonate → (E)-4-(2,4-difluorophenyl)but-3-en-2-one

HRID 906903
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인쇄 미리보기

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HRID 906903 반응식
[F:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.COP([CH2:17][C:18](=[O:20])[CH3:19])(=O)OC.C([O-])([O-])=O.[K+].[K+]>O>[F:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1/[CH:4]=[CH:17]/[C:18](=[O:20])[CH3:19]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 737702,4-DifluorobenzaldehydeHCID 77872Dimethyl (2-oxopropyl)phosphonate

생성물 1

HCID 58310994(E)-4-(2,4-difluorophenyl)but-3-en-2-one수율 79%

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

A two necked flask was charged with 2,4-difluorobenzaldehyde (4.0 g, 28.1 mmol) and (2-oxo-propyl)-phosphonic acid dimethyl ester (5.78 g, 33.0 mmol) and cooled down at at 0° C. K2CO3 (7.62 g, 55.1 mmol) in H2O (14 mL) was added dropwise. Stirring was continued over night at RT. The product was extracted with EtOAc, and the organic phase was dried over Na2SO4. Flash chromatography (SiO2, Heptane/EtOAc 1:3) afforded 4.0 g (79%) of the title compound as alight yellow oil.

후처리

  1. waitwas continued over night at RT
  2. extractionThe product was extracted with EtOAc
  3. dry with materialthe organic phase was dried over Na2SO4

출처 및 근거

ORD 기록
ord-d7fe75a336c5485ba0790a67c405a0ba
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08012998B2

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