Phosphorus oxychloride → 2-Bromo-4-chloropyridin-3-ol

HRID 1846237ノート

反応式

HRID 1846237 の反応式
[Br:1][C:2]1[C:7]([O:8]C)=[C:6]([Cl:10])[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)(Cl)=O.COC1C(=O)C=CNC=1Br>>[Br:1][C:2]1[C:7]([OH:8])=[C:6]([Cl:10])[CH:5]=[CH:4][N:3]=1

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 497615912-Bromo-3-methoxypyridin-4-olHCID 866967432-Bromo-4-chloro-3-methoxypyridine

生成物 1

HCID 722139992-Bromo-4-chloropyridin-3-ol

反応条件

温度
20 °C

実験手順

2-bromo-4-chloro-3-methoxypyridine. Phosphorus oxychloride (10 eq.) and 3-methoxy-2-bromo-4(1H)-pyridone (1 eq.) are stirred at 90° C. for 18 h, concentrated in vacuo, and cooled to 20° C. The residue is treated with ice water and adjusted to pH 12 with 40% NaOH, and the product is extracted into DCM. The residue obtained on evaporation of the combined extracts is distilled at reduced pressure to afford the title compound.

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe residue is treated with ice water
  3. extractionthe product is extracted into DCM
  4. customThe residue obtained on evaporation of the combined extracts
  5. distillationis distilled at reduced pressure

出典と根拠

ORDレコード
ord-6f3984306a1c4420b795d126c90c0480
出典データセット
uspto-grants-2015_02
特許番号
US08952009B2

反応ノート

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