Triethylamine → 8-Methoxy-2-methylquinazoline

HRID 726314노트

반응식

HRID 726314 반응식
Cl[C:2]1[C:11]2[C:6](=[C:7]([O:12][CH3:13])[CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([CH3:14])[N:3]=1.C(N(CC)CC)C>[Pd].C(OCC)(=O)C>[CH3:13][O:12][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:6]=1[N:5]=[C:4]([CH3:14])[N:3]=[CH:2]2

참가 물질

5

반응물 2

HCID 8471TriethylamineHCID 107747604-Chloro-8-methoxy-2-methylquinazoline

생성물 1

HCID 107735698-Methoxy-2-methylquinazoline수율 71.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 4-chloro-8-methoxy-2-methylquinazoline (5.12 g), 10% palladium on carbon (512 mg) and triethylamine (3.72 g) in ethyl acetate (51 ml) was stirred under hydrogen atmosphere for 3 hours. The catalyst was removed by filtration, and the filtrate was concentrated. The residue was dissolved in methylene chloride, and the solution was washed with saturated sodium bicarbonate solution, water and brine, dried over magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (methylene chloride-methanol) to give 8-methoxy-2-methylquinazoline (3.07 g).

후처리

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. dissolutionThe residue was dissolved in methylene chloride
  4. washthe solution was washed with saturated sodium bicarbonate solution, water and brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel column chromatography (methylene chloride-methanol)

출처 및 근거

ORD 기록
ord-9eb41e0b8f00498b90a6f08c3c64cee4
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05708173

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