Acetic Anhydride → N-[6-Chloro-2-(methylsulfanyl)pyrimidin-4-yl]acetamide

HRID 2233839노트

반응식

HRID 2233839 반응식
C(O[C:5](=[O:7])[CH3:6])(=O)C.[Cl:8][C:9]1[N:14]=[C:13]([S:15][CH3:16])[N:12]=[C:11]([NH2:17])[CH:10]=1>C(=O)(O)[O-].[Na+]>[Cl:8][C:9]1[N:14]=[C:13]([S:15][CH3:16])[N:12]=[C:11]([NH:17][C:5](=[O:7])[CH3:6])[CH:10]=1

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 704964-Amino-6-chloro-2-methylthiopyrimidine

생성물 1

HCID 13447564N-[6-Chloro-2-(methylsulfanyl)pyrimidin-4-yl]acetamide수율 120.4%

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

반응 조건

온도
135 °C

실험 절차

Acetic anhydride (10.4 ml, 0.11 mol) was added to 6-chloro-2-(methylthio)pyrimidin-4-amine (2.5 g, 0.01 mol) and the reaction mixture was refluxed at 135° C. for 5 hr. The reaction mixture was cooled to room temperature and basified to pH 7 with saturated sodium bicarbonate solution (20 ml). The mixture was partitioned between EtOAc and water, the organic layer was washed with water and brine, dried over MgSO4 and concentrated to give the title compound (2.62 g).

후처리

  1. customThe mixture was partitioned between EtOAc and water
  2. washthe organic layer was washed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-172ca628a4f245ff8186184e9427b582
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709503B2

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