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

HRID 1981159노트

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HRID 1981159 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 180Acetone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-02f1dd8c79604e7ab433fb06145d14a0
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04512991

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