2-chloro-N-methyl-5-nitropyrimidin-4-amine → 2-Chloro-N4-methylpyrimidine-4,5-diamine

HRID 524044

반응식

HRID 524044 반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH3:9])[C:5]([N+:10]([O-])=O)=[CH:4][N:3]=1>C(O)(=O)C.[Fe]>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH3:9])[C:5]([NH2:10])=[CH:4][N:3]=1

참가 물질

4

반응물 1

HCID 71472322-chloro-N-methyl-5-nitropyrimidin-4-amine

생성물 1

HCID 71471722-Chloro-N4-methylpyrimidine-4,5-diamine수율 69.4%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

반응 조건

온도
60 °C

실험 절차

To a stirred solution of 2-chloro-N-methyl-5-nitropyrimidin-4-amine (1.9 g, 10 mmol) in acetic acid (30 mL) was added iron powder (4 g, 71 mmol), and the suspension mixture was heated to 60° C. for 16 hours. The solvent was removed under reduced pressure, and the residue was diluted by brine and ethyl acetate. The solid was filtered off, and the filtrate was extracted with ethyl acetate (50 mL*12). The organic layers were separated, combined, dried over sodium sulfate, filtered and concentrated to give the title compound (1.1 g, 69%). MS (ES+) C5H7ClN4 requires: 159, 161. found: 160, 162 [M+H]+.

후처리

  1. customThe solvent was removed under reduced pressure
  2. additionthe residue was diluted by brine and ethyl acetate
  3. filtrationThe solid was filtered off
  4. extractionthe filtrate was extracted with ethyl acetate (50 mL*12)
  5. customThe organic layers were separated
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-56951a43107a4a83be3043c748893928
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340514B2

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