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

HRID 1586074ノート

反応式

HRID 1586074 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-411e712361c84e6cb1d5e0ed5dcda5db
出典データセット
uspto-grants-1999_08
特許番号
US05942522

反応ノート

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