2,4,5-Trichloropyrimidine → 3-(2,5-dichloropyrimidin-4-ylamino)pyridin-2(1H)-one

HRID 536331ノート

反応式

HRID 536331 の反応式
[NH2:1][C:2]1[C:3](=[O:8])[NH:4][CH:5]=[CH:6][CH:7]=1.[Cl:9][C:10]1[N:15]=[C:14](Cl)[C:13]([Cl:17])=[CH:12][N:11]=1.C([O-])(O)=O.[Na+]>CO.O>[Cl:9][C:10]1[N:15]=[C:14]([NH:1][C:2]2[C:3](=[O:8])[NH:4][CH:5]=[CH:6][CH:7]=2)[C:13]([Cl:17])=[CH:12][N:11]=1

参加物

6

反応物 3

HCID 2372592,4,5-TrichloropyrimidineHCID 3223533-Amino-2-pyridinolHCID 516892Sodium Bicarbonate

生成物 1

HCID 582551623-(2,5-dichloropyrimidin-4-ylamino)pyridin-2(1H)-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A mixture of 3-aminopyridin-2(1H)-one (99 mg, 0.90 mmol), 2,4,5-trichloropyrimidine (165 mg, 0.90 mmol, 1 equiv.) and NaHCO3 (76 mg, 0.90 mmol, 1 equiv.) in a mixture of MeOH (6 mL) and H2O (3 mL) was stirred at room temperature for 24 h. The resulting precipitate was collected by vacuum filtration and washed with small amounts of MeOH and water, providing the product 3-(2,5-dichloropyrimidin-4-ylamino)pyridin-2(1H)-one; ESMS m/z 257.0 (M+H+).

後処理

  1. filtrationThe resulting precipitate was collected by vacuum filtration
  2. washwashed with small amounts of MeOH and water

出典と根拠

ORDレコード
ord-fa9713ee05d544e2a4f1809f20360022
出典データセット
uspto-grants-2014_10
特許番号
US08859574B2

反応ノート

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