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

HRID 2233839ノート

反応式

HRID 2233839 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
135 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-172ca628a4f245ff8186184e9427b582
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

反応ノート

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