Sulfuric Acid → HCID 67485361、化合物

HRID 533996ノート

反応式

HRID 533996 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([O:10][C:11]2[C:12]([CH3:17])=[N:13][CH:14]=[CH:15][CH:16]=2)[C:5]([C:8]#[N:9])=[N:6][CH:7]=1.S(=O)(=O)(O)[OH:19].[OH-].[Na+]>O>[Br:1][C:2]1[CH:3]=[C:4]([O:10][C:11]2[C:12]([CH3:17])=[N:13][CH:14]=[CH:15][CH:16]=2)[C:5]([C:8]([NH2:9])=[O:19])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 67485726HCID 67485726、化合物

生成物 1

HCID 67485361HCID 67485361、化合物収率 98.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A flask was charged with 5-bromo-3-(2-methylpyridin-3-yloxy)picolinonitrile (60 g, 207 mmol) and sulfuric acid (203 g, 2068 mmol). The reaction was stirred at ambient temperature overnight. Water (500 mL) was added carefully and neutralized using 50% sodium hydroxide to pH 5.0. The mixture was extracted with dichloromethane and ethyl acetate, dried and concentrated to afford 5-bromo-3-(2-methylpyridin-3-yloxy)picolinamide (63.0 g, 204 mmol, 98.9% yield) as yellow solid.

後処理

  1. extractionThe mixture was extracted with dichloromethane and ethyl acetate
  2. customdried
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-c455bb8b59ae47b2b0e9b0c9d474b36d
出典データセット
uspto-grants-2014_10
特許番号
US08853409B2

反応ノート

読み込み中…