Hydroxylamine, O-((4-nitrophenyl)methyl)-, hydrochloride (1:1) → (E)-1-(1,3-benzodioxol-5-yl)-N-[(4-nitrophenyl)methoxy]ethanimine

HRID 41930

反応式

HRID 41930 の反応式
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([C:10](=O)[CH3:11])=[CH:4][C:3]=2[O:2]1.Cl.[N+:14]([C:17]1[CH:25]=[CH:24][C:20]([CH2:21][O:22][NH2:23])=[CH:19][CH:18]=1)([O-:16])=[O:15]>>[N+:14]([C:17]1[CH:18]=[CH:19][C:20]([CH2:21][O:22]/[N:23]=[C:10](/[C:5]2[CH:6]=[CH:7][C:8]3[O:9][CH2:1][O:2][C:3]=3[CH:4]=2)\[CH3:11])=[CH:24][CH:25]=1)([O-:16])=[O:15]

参加物

3

反応物 2

HCID 74967Hydroxylamine, O-((4-nitrophenyl)methyl)-, hydrochloride (1:1)HCID 76622Acetopiperone

生成物 1

HCID 25100245(E)-1-(1,3-benzodioxol-5-yl)-N-[(4-nitrophenyl)methoxy]ethanimine収率 87%

実験手順

3′,4′-Methylenedioxyacetophenone (22) (150 mg, 0.914 mmol) was condensed with compound 19 (206 mg, 1.01 mmol) according to the general procedure II-A defined above. After being heated for 3 h the reaction mixture was cooled and the resulting solid filtered off and washed with cold isopropanol (3.0 mL) to afford the title compound CP30255 (250 mg, 87%) as a yellow solid, m.p. 158.7-160.5° C.

後処理

  1. temperatureAfter being heated for 3 h the reaction mixture
  2. temperaturewas cooled
  3. filtrationthe resulting solid filtered off
  4. washwashed with cold isopropanol (3.0 mL)

出典と根拠

ORDレコード
ord-5536d23c3a294ca286332598e504a048
出典データセット
uspto-grants-2013_09
特許番号
US08536157B2

関連ノート

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