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Water → 4-Cyclopropyl-3-fluoro-2-methoxybenzaldehyde

HRID 2272518
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HRID 2272518 반응식
[CH3:1][O-:2].[Na+].[CH:4]1([C:7]2[CH:14]=[CH:13][C:10]([CH:11]=[O:12])=[C:9](F)[C:8]=2[F:16])[CH2:6][CH2:5]1.O>CO>[CH:4]1([C:7]2[CH:14]=[CH:13][C:10]([CH:11]=[O:12])=[C:9]([O:2][CH3:1])[C:8]=2[F:16])[CH2:6][CH2:5]1
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참가 물질

5

반응물 3

HCID 962WaterHCID 10942334Sodium MethoxideHCID 904235484-Cyclopropyl-2,3-difluorobenzaldehyde

생성물 1

HCID 904232524-Cyclopropyl-3-fluoro-2-methoxybenzaldehyde수율 91.6%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Sodium methoxide (28% methanol solution, 3.43 g) was added at room temperature to a methanol (100 mL) solution of 4-cyclopropyl-2,3-difluorobenzaldehyde (2.16 g), and the mixture was stirred at 70 C for 15 hours in a nitrogen atmosphere. Water was added to the reaction mixture, and methanol was distilled off under reduced pressure. The residue was subjected to extraction with ethyl acetate. The obtained organic layer was washed with water and saturated saline in this order and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (2.11 g)

후처리

  1. distillationwas distilled off under reduced pressure
  2. extractionThe residue was subjected to extraction with ethyl acetate
  3. washThe obtained organic layer was washed with water and saturated saline in this order
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-4aba2023b14a454095d2ad28d556132e
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09120777B2

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