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

HRID 1846237노트

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HRID 1846237 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

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

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온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f3984306a1c4420b795d126c90c0480
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952009B2

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