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Sodium Carbonate → N-(3-nitro-2-pyridinyl)-2-pyrazinemethanamine

HRID 1533954
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HRID 1533954 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.Cl.Cl.[N:13]1[CH:18]=[CH:17][N:16]=[CH:15][C:14]=1[CH2:19][NH2:20].CN(C)C(=O)C.C(=O)([O-])[O-].[Na+].[Na+]>CC(C)CC(=O)C.O>[N+:8]([C:7]1[C:2]([NH:20][CH2:19][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][N:13]=2)=[N:3][CH:4]=[CH:5][CH:6]=1)([O-:10])=[O:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10340Sodium CarbonateHCID 31374DimethylacetamideHCID 796132-Chloro-3-nitropyridineHCID 19911503Pyrazin-2-ylmethanamine dihydrochloride

생성물 1

HCID 17845733N-(3-nitro-2-pyridinyl)-2-pyrazinemethanamine수율 10%

시약·촉매·용매 2

HCID 962Water
용매
HCID 7909Methyl Isobutyl Ketone용매

반응 조건

온도
100 °C

실험 절차

To a stirred solution of 25.4 parts of 2-chloro-3-nitropyridine, 29.5 parts of 2-pyrazinemethanamine dihydrochloride and 235 parts of N,N-dimethylacetamide were added 67.8 parts of sodium carbonate. The reaction mixture was stirred for 1.5 hours at 100° C. The reaction mixture was poured into water and 4-methyl-2-pentanone. The whole was filtered twice over diatomaceous earth and the layers were separated. The organic layer was dried, filtered and evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 3.6 parts (10%) of N-(3-nitro-2-pyridinyl)-2-pyrazinemethanamine (int. 27).

후처리

  1. filtrationThe whole was filtered twice over diatomaceous earth
  2. customthe layers were separated
  3. customThe organic layer was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was crystallized from acetonitrile
  7. filtrationThe product was filtered off
  8. customdried

출처 및 근거

ORD 기록
ord-4d5aa872477f4973a8e725d49ce781e4
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05086056

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