Hydrogen Peroxide → HCID 59464117、化合物

HRID 1713877ノート

反応式

HRID 1713877 の反応式
OO.FC(F)(F)C(OC(=O)C(F)(F)F)=[O:6].[Cl:16][C:17]1[N:22]=[CH:21][C:20]([CH2:23][C:24]([O:26][CH3:27])=[O:25])=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[Cl:16][C:17]1[N+:22]([O-:6])=[CH:21][C:20]([CH2:23][C:24]([O:26][CH3:27])=[O:25])=[CH:19][CH:18]=1

参加物

6

反応物 4

HCID 784Hydrogen PeroxideHCID 9845Trifluoroacetic anhydrideHCID 11430Potassium CarbonateHCID 53419528Methyl 2-(6-chloropyridin-3-yl)acetate

生成物 1

HCID 59464117HCID 59464117、化合物収率 44%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Hydrogen peroxide (0.409 mL of a 30% aqueous solution, 3.6 mmol) was added slowly to a stirred solution of trifluoroacetic anhydride (0.915 mL, 6.55 mmol) in DCM (5 mL) with heating under reflux. After 30 min, methyl (6-chloropyridin-3-yl)acetate (Indian Journal of Chemistry, Section B: Organic Chemistry Including Medicinal Chemistry (2004), 43B(4), 864) (608 mg, 3.28 mmol) was added as a solution in DCM (5 mL). The reaction mixture was stirred under reflux for 1 h and then allowed to cool with stirring for 16 h. Solid potassium carbonate was added until there was no more effervescence then the mixture was filtered, concentrated by evaporation and the resultant oil was triturated with Et2O to give the title compound (291 mg, 44%) as a solid; 1H NMR δ 3.64 (s, 3H), 3.79 (s, 2H), 7.30 (d, 1H), 7.75 (d, 1H), 8.45 (s, 1H); MS m/e MH+ 202.

後処理

  1. temperaturewith heating
  2. temperatureunder reflux
  3. temperatureunder reflux for 1 h
  4. temperatureto cool
  5. stirringwith stirring for 16 h
  6. filtrationthe mixture was filtered
  7. concentrationconcentrated by evaporation
  8. customthe resultant oil was triturated with Et2O

出典と根拠

ORDレコード
ord-97c365d1229a4cd0bc4dab6cd48547a3
出典データセット
uspto-grants-2010_09
特許番号
US07795283B2

反応ノート

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