Acetic Anhydride → N-(2,6-dichloropyrimidin-4-yl)acetamide

HRID 2233809

反応式

HRID 2233809 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([Cl:9])[N:3]=1.C([O-])(O)=O.[Na+].[C:15](OC(=O)C)(=[O:17])[CH3:16]>>[Cl:9][C:4]1[N:3]=[C:2]([NH:1][C:15](=[O:17])[CH3:16])[CH:7]=[C:6]([Cl:8])[N:5]=1

参加物

4

反応物 3

HCID 7918Acetic AnhydrideHCID 823874-Pyrimidinamine, 2,6-dichloro-HCID 516892Sodium Bicarbonate

生成物 1

HCID 4713752N-(2,6-dichloropyrimidin-4-yl)acetamide収率 80%

実験手順

4-Amino-2,6-dichloropyrimidine (500 mg, 3.05 mmol) was refluxed in acetic anhydride (10 ml) for 3 h. Upon cooling to room temperature, the reaction mixture was cooled in an ice bath and basified to pH 8 with 10% aqueous NaHCO3. The phases were separated, and the aqueous portion was extracted twice with EtOAc. The combined organic portions were dried over Na2SO4, filtered, and concentrated to give an off-white solid (503.7 mg, 2.44 mmol, 80% yield).

後処理

  1. temperaturethe reaction mixture was cooled in an ice bath
  2. customThe phases were separated
  3. extractionthe aqueous portion was extracted twice with EtOAc
  4. dry with materialThe combined organic portions were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c1a94b172384472c8dda843e419df92c
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

関連ノート

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