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

HRID 2091929ノート

反応式

HRID 2091929 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) is stirred at room temperature for 24 h. The resulting precipitate is 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 is collected by vacuum filtration
  2. washwashed with small amounts of MeOH and water

出典と根拠

ORDレコード
ord-f7e26e2eb49a4699a7efb809cb220cab
出典データセット
uspto-grants-2013_05
特許番号
US08440681B2

反応ノート

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