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

HRID 968604ノート

反応式

HRID 968604 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-841955b274844056ab2b59676c656c06
出典データセット
uspto-grants-2007_12
特許番号
US07304059B2

反応ノート

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