Hydroxyamine hydrochloride → HCID 85177110, 화합물

HRID 1451094노트

반응식

HRID 1451094 반응식
[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]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 12464019HCID 12464019, 화합물

생성물 1

HCID 85177110HCID 85177110, 화합물수율 53%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0e765bfd74ed45f29bc9e6a2c809baaf
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602277

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