2,6-Lutidine → 7-Bromo-4-chloro-2-(chloromethyl)quinazoline

HRID 968604노트

반응식

HRID 968604 반응식
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[NH:7][C:8]([CH2:12][Cl:13])=[N:9]2)=[CH:4][CH:3]=1.N1C(C)=CC=CC=1C.P(Cl)(Cl)([Cl:25])=O>COCCOC>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([Cl:25])=[N:7][C:8]([CH2:12][Cl:13])=[N:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 79372,6-LutidineHCID 24813Phosphorus oxychlorideHCID 1356820607-Bromo-2-(chloromethyl)quinazolin-4-ol

생성물 1

HCID 220301087-Bromo-4-chloro-2-(chloromethyl)quinazoline

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

Heat a mixture of 7-bromo-2-chloromethyl-3H-quinazolin-4-one (5 g, 18.2 mmol), 2,6-lutidine (5 g), and phosphorus oxychloride (5 mL) in 1,2-dimethoxyethane (500 mL) at 80° C. for 16 hours. Cool the mixture to room temperature and fully evaporate the mixture, then dilute with ether and wash with water. Dry the solvent (Na2SO4) and evaporate the ether to obtain 7-bromo-4-chloro-2-chloromethylquinazoline (3.5 g) as a yellow solid.

후처리

  1. temperatureHeat
  2. customfully evaporate the mixture
  3. additiondilute with ether
  4. washwash with water
  5. dry with materialDry the solvent (Na2SO4)
  6. customevaporate the ether

출처 및 근거

ORD 기록
ord-841955b274844056ab2b59676c656c06
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07304059B2

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