HCID 22024596、化合物 → HCID 22024494、化合物

HRID 500989ノート

反応式

HRID 500989 の反応式
[Cl:1][C:2]1[C:3]2[N:4]([C:8]([CH:13]([OH:17])[CH2:14][CH2:15][CH3:16])=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[CH:6][N:7]=1>C(OCC)(=O)C.C(Cl)Cl.[O-2].[Mn+4].[O-2]>[Cl:1][C:2]1[C:3]2[N:4]([C:8]([C:13](=[O:17])[CH2:14][CH2:15][CH3:16])=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[CH:6][N:7]=1

参加物

5

反応物 1

HCID 22024596HCID 22024596、化合物

生成物 1

HCID 22024494HCID 22024494、化合物

試薬・触媒・溶媒 3

HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

The resulting 1-(8-chloro-2-ethylimidazo[1,2-a]pyrazin-3-yl)-1-butanol was dissolved in ethyl acetate (4 mL) and methylene chloride (1 mL), then activated manganese (IV) oxide (3 g) was added thereto, and the mixture was heated under stirring at 60° C. for 5 hours. After being allowed to cool, the reaction mixture was filtered and washed with ethyl acetate, and then the filtrates were combined and evaporated. The resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3) to give the title compound (226 mg) as white crystals.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto cool
  3. filtrationthe reaction mixture was filtered
  4. washwashed with ethyl acetate
  5. customevaporated
  6. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

出典と根拠

ORDレコード
ord-8a75eb283eea4e508ba53ae6f570740d
出典データセット
uspto-grants-2010_08
特許番号
US07772249B2

反応ノート

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