Sulfuric Acid → 3-(2,6-Dimethylpyridin-3-yloxy)-5-bromopicolinamide

HRID 1523559노트

반응식

HRID 1523559 반응식
[Br:1][C:2]1[CH:3]=[C:4]([O:10][C:11]2[C:12]([CH3:18])=[N:13][C:14]([CH3:17])=[CH:15][CH:16]=2)[C:5]([C:8]#[N:9])=[N:6][CH:7]=1.S(=O)(=O)(O)[OH:20].[OH-].[Na+]>>[CH3:18][C:12]1[C:11]([O:10][C:4]2[C:5]([C:8]([NH2:9])=[O:20])=[N:6][CH:7]=[C:2]([Br:1])[CH:3]=2)=[CH:16][CH:15]=[C:14]([CH3:17])[N:13]=1

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 674864525-Bromo-3-(2,6-dimethylpyridin-3-yloxy)picolinonitrile

생성물 1

HCID 679943583-(2,6-Dimethylpyridin-3-yloxy)-5-bromopicolinamide수율 92%

실험 절차

To 5-bromo-3-(2,6-dimethylpyridin-3-yloxy)picolinonitrile (25 g, 82 mmol) was added concentrated sulfuric acid (25 ml) and the mixture stirred at ambient temperature over night. The mixture was poured onto ice (500 ml) and the aqueous mixture neutralized using 50% NaOH. A solid formed at pH 7. The solid was collected and dried in vacuo to afford 3-(2,6-dimethylpyridin-3-yloxy)-5-bromopicolinamide (24.2 g, 92%).

후처리

  1. additionThe mixture was poured onto ice (500 ml)
  2. customA solid formed at pH 7
  3. customThe solid was collected
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-4de8c11f9085406d8a6bc8546e04adcd
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079890B2

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