Water → HCID 178520452、化合物

HRID 967753ノート

反応式

HRID 967753 の反応式
C[N:2]([CH:4]=[N:5][C:6](=[O:15])[CH:7]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)C.Cl.N[OH:18].[OH-].[Na+].O>C(O)(=O)C>[OH:18][NH:2][CH:4]=[N:5][C:6](=[O:15])[CH:7]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 3745097N-[(Dimethylamino)methylene]-cinnamamide

生成物 1

HCID 178520452HCID 178520452、化合物収率 90%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
5 °C

実験手順

N-[(Dimethylamino)methylene]-cinnamamide (1.0 g, 5.0 mmol) was added to a solution of hydroxylamine hydrochloride (415 mg, 6.0 mmol) in acetic acid (5 mL of 70% aqueous) and aqueous NaOH (1.2 mL, 5 M, 6.0 mmol). After stirring for 1.5 h water (5 mL) was added, and the reaction mixture was cooled to 5° C. in an ice bath. The solution was partitioned between ethyl acetate and water, and the organics were dried over Na2SO4, then concentrated in vacuo to afford N-[(hydroxyamino)methylene]-cinnamamide (850 mg, 90%). This material was carried on to the next step without further purification.

後処理

  1. additionwas added
  2. customThe solution was partitioned between ethyl acetate and water
  3. dry with materialthe organics were dried over Na2SO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8d28f91bda164931a76ed093a67b4430
出典データセット
uspto-grants-2005_10
特許番号
US06956049B1

反応ノート

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