Methyl iodide → HCID 67299926, 화합물

HRID 1260299노트

반응식

HRID 1260299 반응식
[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]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 67299931HCID 67299931, 화합물

생성물 1

HCID 67299926HCID 67299926, 화합물수율 27%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c78530ccd1294539a1ce4c5147b390f8
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08470820B2

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