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

HRID 2084703ノート

反応式

HRID 2084703 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6a87eb3f1ef54249ba69d33298b08d10
出典データセット
uspto-grants-2004_04
特許番号
US06716991B1

反応ノート

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