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HCID 20463835, 화합물 → 5,6-Dichloro-3-[(2-hydroxyethyl)amino]pyrazine-2-carbaldehyde

HRID 325608
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HRID 325608 반응식
[Cl:1][C:2]1[N:3]=[C:4]([CH2:13][OH:14])[C:5]([NH:9][CH2:10][CH2:11][OH:12])=[N:6][C:7]=1[Cl:8]>CC(C)=O.[O-2].[O-2].[Mn+4]>[Cl:1][C:2]1[N:3]=[C:4]([CH:13]=[O:14])[C:5]([NH:9][CH2:10][CH2:11][OH:12])=[N:6][C:7]=1[Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 20463835HCID 20463835, 화합물

생성물 1

HCID 204638365,6-Dichloro-3-[(2-hydroxyethyl)amino]pyrazine-2-carbaldehyde수율 71.5%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매3회HCID 180Acetone용매

실험 절차

A mixture of 5,6-dichloro-3-hydroxymethyl-2-(2-hydroxyethyl)aminopyrazine (38 mg; 0.00016 Mol), prepared as in Step C above, and manganese dioxide (12 mg) was stirred at room temperature for 2.5 hours. Another 24 mg of manganese dioxide was added and stirring was continued for another 5 hours. The manganese dioxide was filtered off, and the precipitate was washed well with acetone. The crude reaction mixture dissolved in 1.5 l of acetone and 36 mg of manganese dioxide was added, followed by stirring at room temperature for 3.5 hours. The manganese dioxide was filtered off, and the precipitate was washed twice with acetone. The filtrate was concentrated under vacuum and passed through a silica gel column, eluting with dichloromethane, then 1:1 ethyl acetate/dichloromethane, to give the title compound (27 mg). Elemental Analysis for C7H7O2N3Cl2 :

후처리

  1. stirringstirring
  2. waitwas continued for another 5 hours
  3. filtrationThe manganese dioxide was filtered off
  4. washthe precipitate was washed well with acetone
  5. customThe crude reaction mixture
  6. stirringby stirring at room temperature for 3.5 hours
  7. filtrationThe manganese dioxide was filtered off
  8. washthe precipitate was washed twice with acetone
  9. concentrationThe filtrate was concentrated under vacuum
  10. washeluting with dichloromethane

출처 및 근거

ORD 기록
ord-a665aae9153149b080c5fd4e9e4a120a
출처 데이터셋
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04442097

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