Phosphorus oxychloride → 2-Chloro-6-methoxyquinazoline

HRID 639354ノート

反応式

HRID 639354 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[C:8](O)[N:7]=[CH:6]2.P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:8]1[N:7]=[CH:6][C:5]2[C:10](=[CH:11][CH:12]=[C:3]([O:2][CH3:1])[CH:4]=2)[N:9]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178488027HCID 178488027、化合物

生成物 1

HCID 592548522-Chloro-6-methoxyquinazoline収率 90%

実験手順

6-methoxyquinazolin-2-ol (1eq) and phosphorus oxychloride (2-10eq) was refluxed for 2 hours. The reaction mixture was concentrated and neutralized with sodium carbonate, which was then filtered off. The concentrate was partitioned between ethyl acetate and water. The organic layer was then washed with brine dried and concentrated. The crude was subjected to column chromatography (10% Acetone in hexane) to afford 2-chloro-6-methoxyquinazoline as a beige color solid in 90% yield.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. filtrationwas then filtered off
  3. customThe concentrate was partitioned between ethyl acetate and water
  4. washThe organic layer was then washed with brine
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-47bd76c8e845491bb1fa6d0fb243495c
出典データセット
uspto-grants-2010_04
特許番号
US07691866B2

反応ノート

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