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

HRID 36048ノート

反応式

HRID 36048 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-a40c1a07051a426abca2e4f03fe4e1e8
出典データセット
uspto-grants-1995_05
特許番号
US05412104

反応ノート

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