O-((2E)-3-Chloro-2-propen-1-yl)hydroxylamine → HCID 178458080、化合物

HRID 1606868ノート

反応式

HRID 1606868 の反応式
[CH3:1][N:2]1[C:6]([CH:7]2[CH2:12][C:11](=[O:13])[CH:10]([C:14](=O)[CH2:15][CH3:16])[C:9](=[O:18])[CH2:8]2)=[CH:5][C:4]([CH3:19])=[N:3]1.[Cl:20]/[CH:21]=[CH:22]/[CH2:23][O:24][NH2:25]>CO>[Cl:20][CH:21]=[CH:22][CH2:23][O:24]/[N:25]=[C:14](/[CH:10]1[C:11](=[O:13])[CH2:12][CH:7]([C:6]2[N:2]([CH3:1])[N:3]=[C:4]([CH3:19])[CH:5]=2)[CH2:8][C:9]1=[O:18])\[CH2:15][CH3:16]

参加物

4

反応物 2

HCID 158058O-((2E)-3-Chloro-2-propen-1-yl)hydroxylamineHCID 145362605-(1,3-dimethyl-1H-pyrazol-5-yl)-2-propionylcyclohexane-1,3-dione

生成物 1

HCID 178458080HCID 178458080、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 10 ml of a solution of 5.60 g (21.3 mmols) of 5-(1,3-dimethyl-1H-pyrazol-5-yl)-2-propionylcyclohexane-1,3-dione in methanol was added 57 ml (21.7 mmols) of 0.38 mol ethanolic solution of (E)-3-chloro-2-propenyloxyamine. The mixture was reacted for 10 hours with stirring. After completion of the reaction, the reaction mixture was concentrated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane:ethyl acetate=2:1) to give 6.84 g of the product.

後処理

  1. customThe mixture was reacted for 10 hours
  2. customAfter completion of the reaction
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. customThe resulting crude product was purified by silica gel column chromatography (hexane:ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-517fdeb7e1764c90831793729aa18792
出典データセット
uspto-grants-1989_09
特許番号
US04863504

反応ノート

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