Methyl iodide → HCID 67299926、化合物

HRID 1260299ノート

反応式

HRID 1260299 の反応式
[Br:1][C:2]1[C:3]([C:11]([OH:13])=[O:12])=[N:4][C:5]([CH2:8][O:9][CH3:10])=[N:6][CH:7]=1.[C:14]([O-])([O-])=O.[Cs+].[Cs+].CI>CC(C)=O>[CH3:14][O:12][C:11]([C:3]1[C:2]([Br:1])=[CH:7][N:6]=[C:5]([CH2:8][O:9][CH3:10])[N:4]=1)=[O:13]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 67299931HCID 67299931、化合物

生成物 1

HCID 67299926HCID 67299926、化合物収率 27%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 5-bromo-2-methoxymethyl-pyrimidine-4-carboxylic acid (2.5 g, 10.1 mmol) in acetone (100 ml) was added Cs2CO3 (19.8 g, 60.7 mmol) followed by methyliodide (3.8 ml, 60.7 mmol). The mixture was heated to reflux for 8 h. The reaction mixture was then filtered, and the filtrate was evaporated. The crude material was purified by silica gel chromatography using a ethyl acetate/hexane eluent to yield 700 mg (27%) of the title compound as yellow oil.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 8 h
  3. filtrationThe reaction mixture was then filtered
  4. customthe filtrate was evaporated
  5. customThe crude material was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-c78530ccd1294539a1ce4c5147b390f8
出典データセット
uspto-grants-2013_06
特許番号
US08470820B2

反応ノート

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