4-Ethenylbenzonitrile → N-Hydroxy-4-vinyl-benzamidine

HRID 1948514

反応式

HRID 1948514 の反応式
[CH:1]([C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=1)=[CH2:2].Cl.[NH2:12][OH:13].C(=O)(O)[O-].[Na+]>CC(O)C.C(OCC)(=O)C>[OH:13][N:12]=[C:7]([NH2:8])[C:6]1[CH:9]=[CH:10][C:3]([CH:1]=[CH2:2])=[CH:4][CH:5]=1

参加物

6

反応物 3

HCID 769674-EthenylbenzonitrileHCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 74440816N-Hydroxy-4-vinyl-benzamidine収率 96.7%

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 4-vinylbenzonitrile (4.36 g, 33.8 mmol) and hydroxylamine hydrochloride (4.69 g, 67.5 mmol) in 2-propanol (50 mL) was added sodium bicarbonate (11.34 g, 135 mmol). The reaction mixture was heated at 80° C. for 2 hours. The reaction mixture was diluted with ethyl acetate and washed with water. The organic layer was dried MgSO4, filtered, and concentrated to yield 5.3 g of N′-hydroxy-4-vinylbenzimidamide. MS (m+1)=163. HPLC Peak RT=0.53 minutes (Analytical Method B).

後処理

  1. washwashed with water
  2. filtrationfiltered
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-9cd4ae3661cf457e8a0ec17500c06b94
出典データセット
uspto-grants-2013_03
特許番号
US08399451B2

関連ノート

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