Sulfuric Acid → HCID 67485361, 화합물

HRID 533996노트

반응식

HRID 533996 반응식
[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

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 67485726HCID 67485726, 화합물

생성물 1

HCID 67485361HCID 67485361, 화합물수율 98.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c455bb8b59ae47b2b0e9b0c9d474b36d
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853409B2

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