Hydrochloric Acid → 3-Bromoisonicotinic Acid Hydrochloride

HRID 31392

反応式

HRID 31392 の反応式
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]

参加物

4

反応物 3

HCID 313Hydrochloric Acid2 回HCID 8857Ethyl AcetateHCID 107076353-Bromo-N-phenyl-4-pyridinecarboxamide

生成物 1

HCID 684306873-Bromoisonicotinic Acid Hydrochloride

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4e62c98afe98442b8aeb7a93262819b2
出典データセット
uspto-grants-2008_09
特許番号
US07425639B2

関連ノート

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