Isobutyl iodide → 6-Chloro-1-isobutyl-3-methylpyrimidine-2,4(1H,3H)-dione

HRID 81405

반응식

HRID 81405 반응식
[Cl:1][C:2]1[NH:7][C:6](=[O:8])[N:5]([CH3:9])[C:4](=[O:10])[CH:3]=1.[CH2:11](I)[CH:12]([CH3:14])[CH3:13].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[N:7]([CH2:11][CH:12]([CH3:14])[CH3:13])[C:6](=[O:8])[N:5]([CH3:9])[C:4](=[O:10])[CH:3]=1

참가 물질

5

반응물 3

HCID 10556Isobutyl iodide2회HCID 11430Potassium CarbonateHCID 961416-chloro-3-methylpyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 52825666-Chloro-1-isobutyl-3-methylpyrimidine-2,4(1H,3H)-dione수율 52%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

A mixture of 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione (3 g, 18.8 mmol), isobutyl iodide (5 mL, 43.5 mmol) and potassium carbonate (5.3 g, 38.4 mmol) in anhydrous DMF (200 mL) is heated at 50° C. for 8 hours. Additional isobutyl iodide (4.3 mL, 37.5 mmol) is added, and the reaction mixture heated at 50° C. for 24 hours. After hot filtration, the filtrate is evaporated to dryness under reduced pressure. The obtained oil is further purified by silica-gel flash chromatography to give 2.1 g of pure product (Yield: 52%).

후처리

  1. temperaturethe reaction mixture heated at 50° C. for 24 hours
  2. filtrationAfter hot filtration
  3. customthe filtrate is evaporated to dryness under reduced pressure
  4. customThe obtained oil is further purified by silica-gel flash chromatography

출처 및 근거

ORD 기록
ord-a010378496ce4d479c7bed4cc77af8c5
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846693B2

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