Phosphorus oxychloride → 8-Bromo-2-chloro-6-fluoroquinazoline

HRID 2079635ノート

反応式

HRID 2079635 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([F:13])[CH:5]=[C:6]2[C:11]=1[N:10]=[C:9](O)[N:8]=[CH:7]2.P(Cl)(Cl)([Cl:16])=O>>[Br:1][C:2]1[CH:3]=[C:4]([F:13])[CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([Cl:16])[N:8]=[CH:7]2

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178517532HCID 178517532、化合物

生成物 1

HCID 591992998-Bromo-2-chloro-6-fluoroquinazoline収率 89%

実験手順

A 0.5M suspension of 8-bromo-6-fluoroquinazolin-2-ol in phosphorus oxychloride was heated to 110° C. in an oil bath. The suspension was turned to a brown color solution in 20 min. LCMS data showed that the reaction was complete after 1 h. The phosphorus oxychloride was removed by concentration. The residue was mixed with ice water, and adjusted pH to 7 by adding sodium bicarbonate. Reaction mixture was extracted with ethyl acetate. Combined organic phase was washed with water, brine, dried over sodium sulfate and concentrated to give desired product in 89% yield. ES/MS m/z 261/263 (MH+).

後処理

  1. waitwas complete after 1 h
  2. customThe phosphorus oxychloride was removed by concentration
  3. additionThe residue was mixed with ice water
  4. additionby adding sodium bicarbonate
  5. customReaction mixture
  6. extractionwas extracted with ethyl acetate
  7. washCombined organic phase was washed with water, brine
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-df2e807f2f7f43469d34537dc5ab5437
出典データセット
uspto-grants-2011_04
特許番号
US07932262B2

反応ノート

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