Hydroxyamine hydrochloride → HCID 85177110、化合物

HRID 1451094ノート

反応式

HRID 1451094 の反応式
[C:1]([NH:4][C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[CH:7][C:6]=1[CH:15]=O)(=[O:3])[CH3:2].Cl.[NH2:18][OH:19]>C(OCC)(=O)C>[C:1]([NH:4][C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[CH:7][C:6]=1[CH:15]=[N:18][OH:19])(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 12464019HCID 12464019、化合物

生成物 1

HCID 85177110HCID 85177110、化合物収率 53%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of methyl 4-acetylamino-3-formylbenzoate (Gassman, P. G.; Drews, H. R. J. Am. Chem. Soc. 1978, 100, 7600-7610) (0.442 g, 0.002 mol) and hydroxylamine hydrochloride (0.174 g, 0.0025 mol) in ethyl acetate (10 mL) was heated at reflux for 16 h. White precipitate formed which was removed by filtration and the filtrate was concentrated to dryness. The residue was recrystallized from ethyl acetate-hexane to give 0.25 g (53%) of methyl 4-acetylamino-3-[(N-hydroxylimino)methyl]benzoate as a pale yellow powder, mp 200°-203° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. customWhite precipitate formed which
  4. customwas removed by filtration
  5. concentrationthe filtrate was concentrated to dryness
  6. customThe residue was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-0e765bfd74ed45f29bc9e6a2c809baaf
出典データセット
uspto-grants-1997_02
特許番号
US05602277

反応ノート

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