Hydrochloric Acid → 1-(1,3-Benzodioxol-5-yl)-4,4-difluoro-1,3-butanedione

HRID 2084703노트

반응식

HRID 2084703 반응식
[F:1][CH:2]([F:8])[C:3](OCC)=[O:4].C[O-].[Na+].[CH2:12]1[O:20][C:19]2[CH:18]=[CH:17][C:16]([C:21](=[O:23])[CH3:22])=[CH:15][C:14]=2[O:13]1.Cl>CCOCC>[O:20]1[C:19]2[CH:18]=[CH:17][C:16]([C:21](=[O:23])[CH2:22][C:3](=[O:4])[CH:2]([F:8])[F:1])=[CH:15][C:14]=2[O:13][CH2:12]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 9961Ethyl difluoroacetateHCID 76622AcetopiperoneHCID 10942334Sodium Methoxide

생성물 1

HCID 120809131-(1,3-Benzodioxol-5-yl)-4,4-difluoro-1,3-butanedione

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Ethyl difluoroacetate (1.72 g, 11 mmol) was dissolved in ether (25 mL). To the stirred solution was added 25% sodium methoxide (2.38 g, 11 mmol) followed by 3′,4′-(methylenedioxy)acetophenone (1.64 g, 10 mmol). After stirring 16 hours, 1N HCl (25 mL) was added. The organic layer was collected and washed with water (2×25 mL), dried over magnesium sulfate, filtered, and concentrated. The resulting crude dione was used in the next step without further purification of characterization.

후처리

  1. customThe organic layer was collected
  2. washwashed with water (2×25 mL)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe resulting crude dione was used in the next step without further purification of characterization

출처 및 근거

ORD 기록
ord-6a87eb3f1ef54249ba69d33298b08d10
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06716991B1

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