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

HRID 524044

反応式

HRID 524044 の反応式
[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

参加物

4

反応物 1

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

生成物 1

HCID 71471722-Chloro-N4-methylpyrimidine-4,5-diamine収率 69.4%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-56951a43107a4a83be3043c748893928
出典データセット
uspto-grants-2016_05
特許番号
US09340514B2

関連ノート

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