Hydrochloric Acid → 3-Bromoisonicotinic Acid Hydrochloride

HRID 2234266

반응식

HRID 2234266 반응식
C1(N[C:8](=[O:16])[C:9]2[CH:14]=[CH:13][N:12]=[CH:11][C:10]=2[Br:15])C=CC=CC=1.[ClH:17].C(OCC)(=[O:20])C>>[ClH:17].[Br:15][C:10]1[CH:11]=[N:12][CH:13]=[CH:14][C:9]=1[C:8]([OH:16])=[O:20]

참가 물질

4

반응물 3

HCID 313Hydrochloric Acid2회HCID 8857Ethyl AcetateHCID 107076353-Bromo-N-phenyl-4-pyridinecarboxamide

생성물 1

HCID 684306873-Bromoisonicotinic Acid Hydrochloride

실험 절차

To an RBF equipped with a condenser and outfitted with a heating mantle was placed the N-phenyl-3-bromo-isonicotinamide (34 g, 0.123 mol) and 200 ml of 25% HCl. The reaction was left to stir for 3 days. The mixture was cooled to room temperature, and diluted with ethyl acetate. The aqueous layer was extracted and the two layers separated. To the aqueous layer, solid Na2CO3 was added until the pH˜4-5 and a dark oil layer appeared. This was then diluted and extracted with ethyl acetate. The two layers were separated and the aqueous layer was concentrated under reduced pressure to give an off-white solid. To this 100 ml of 2M HCl was added and the solids collected. The off-white solids were placed in a vacuum oven at 60° C. overnight. Yield: 22.4 g (76% th).

후처리

  1. customTo an RBF equipped with a condenser
  2. waitThe reaction was left
  3. extractionThe aqueous layer was extracted
  4. customthe two layers separated
  5. additionTo the aqueous layer, solid Na2CO3 was added until the pH˜4-5
  6. additionThis was then diluted
  7. extractionextracted with ethyl acetate
  8. customThe two layers were separated
  9. concentrationthe aqueous layer was concentrated under reduced pressure
  10. customto give an off-white solid
  11. customthe solids collected
  12. waitThe off-white solids were placed in a vacuum oven at 60° C. overnight

출처 및 근거

ORD 기록
ord-ea7f223eb6724e26ad1ed216860f8d89
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709677B2

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