Hydroxyamine hydrochloride → 1-hexyl-3-oximinomethyl-4-methoxy-6-methyl-2(1H)-quinolinone

HRID 36048노트

반응식

HRID 36048 반응식
[CH2:1]([N:7]1[C:16]2[C:11](=[CH:12][C:13]([CH3:17])=[CH:14][CH:15]=2)[C:10]([O:18][CH3:19])=[C:9]([CH:20]=O)[C:8]1=[O:22])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Cl.[NH2:24][OH:25].C([O-])(=O)C.[Na+]>CO.O>[CH2:1]([N:7]1[C:16]2[C:11](=[CH:12][C:13]([CH3:17])=[CH:14][CH:15]=2)[C:10]([O:18][CH3:19])=[C:9]([CH:20]=[N:24][OH:25])[C:8]1=[O:22])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 152333661-hexyl-3-formyl-4-methoxy-6-methyl-2(1H)-quinolinone

생성물 1

HCID 731897501-hexyl-3-oximinomethyl-4-methoxy-6-methyl-2(1H)-quinolinone

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A solution of 1-hexyl-3-formyl-4-methoxy-6-methyl-2(1H)-quinolinone (Step (2) of Example 1, 1 g), hydroxylamine hydrochloride (0.3 g) and sodium acetate (0.3 g) in methanol (20 ml) was stirred for 3hrs. The mixture was then diluted with water and extracted with methylene chloride. The extracts were dried, evaporated and the resulting solid was crystallized from ether-hexane to give 1 -hexyl-3-oximinomethyl-4-methoxy-6-methyl-2(1H)-quinolinone. That the expected product was obtained was confirmed by the spectral data: MS: m/e 316 (M+); NMR (CDCl3): δ3.98 (s, 3H, OCH3), 8.54 (s, 1H, CH=N).

후처리

  1. extractionextracted with methylene chloride
  2. customThe extracts were dried
  3. customevaporated
  4. customthe resulting solid was crystallized from ether-hexane

출처 및 근거

ORD 기록
ord-a40c1a07051a426abca2e4f03fe4e1e8
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05412104

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