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

HRID 2233809

반응식

HRID 2233809 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c1a94b172384472c8dda843e419df92c
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709503B2

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