2-Amino-5,6-dichloro-3-(1-hydroxyethyl)pyrazine → 1-(3-Amino-5,6-dichloropyrazin-2-yl)ethanone

HRID 1981159ノート

反応式

HRID 1981159 の反応式
[NH2:1][C:2]1[C:7]([CH:8]([OH:10])[CH3:9])=[N:6][C:5]([Cl:11])=[C:4]([Cl:12])[N:3]=1>CC(C)=O.[O-2].[O-2].[Mn+4]>[C:8]([C:7]1[C:2]([NH2:1])=[N:3][C:4]([Cl:12])=[C:5]([Cl:11])[N:6]=1)(=[O:10])[CH3:9]

参加物

4

反応物 1

HCID 203998652-Amino-5,6-dichloro-3-(1-hydroxyethyl)pyrazine

生成物 1

HCID 203998601-(3-Amino-5,6-dichloropyrazin-2-yl)ethanone

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 180Acetone溶媒

実験手順

In 6 ml of acetone there was dissolved 90 mg of 2-amino-5,6-dichloro-3-(1-hydroxyethyl)pyrazine prepared in Step A above, after which there was added 360 mg of manganese dioxide, and the reaction mixture was stirred for 3 days at room temperature. The manganese dioxide was filtered off, and the precipitate washed three times with acetone, and then filtered. The filtrate was concentrated under vacuum and passed through a silica gel column, then eluted first with hexane, followed by 10% dichloromethane in hexane, with product in the first three fractions (53 mg).

後処理

  1. filtrationThe manganese dioxide was filtered off
  2. washthe precipitate washed three times with acetone
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under vacuum
  5. washeluted first with hexane

出典と根拠

ORDレコード
ord-02f1dd8c79604e7ab433fb06145d14a0
出典データセット
uspto-grants-1985_04
特許番号
US04512991

反応ノート

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