Dimethylformamide → HCID 67778586、化合物

HRID 1026279

反応式

HRID 1026279 の反応式
[OH:1][C:2]1[CH:6]=[C:5]([C:7]([O:9][CH3:10])=[O:8])[O:4][N:3]=1.[F:11][CH2:12][CH:13]1[CH2:15][O:14]1.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>O>[F:11][CH2:12][CH:13]([OH:14])[CH2:15][O:1][C:2]1[CH:6]=[C:5]([C:7]([O:9][CH3:10])=[O:8])[O:4][N:3]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 104181,2-Epoxy-3-fluoropropaneHCID 11430Potassium CarbonateHCID 178498603HCID 178498603、化合物

生成物 1

HCID 67778586HCID 67778586、化合物収率 20.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of methyl 3-hydroxyisoxazole-5-carboxylate (1.88 g), 2-(fluoromethyl)oxirane (1.00 g), potassium carbonate (1.82 g) and DMF (2 mL) was stirred at room temperature for 2 hr, and then at 70° C. overnight. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound as a white powder (585 mg).

後処理

  1. customat 70° C.
  2. customovernight
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe obtained organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-3d3184b8ecaf47eea6539dc31b83b13a
出典データセット
uspto-grants-2014_05
特許番号
US08729102B2

関連ノート

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