Hydroxyamine hydrochloride → 4-(5-Isoxazolyl)benzonitrile

HRID 1370073

反応式

HRID 1370073 の反応式
Cl.NO.[C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12](=[O:18])[CH:13]=[CH:14][N:15](C)C)=[CH:8][CH:7]=1)#[N:5]>CO.O>[O:18]1[C:12]([C:9]2[CH:10]=[CH:11][C:6]([C:4]#[N:5])=[CH:7][CH:8]=2)=[CH:13][CH:14]=[N:15]1

参加物

5

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 28059521-(4-Cyanophenyl)3-dimethylaminopropen-1-one

生成物 1

HCID 185170264-(5-Isoxazolyl)benzonitrile収率 89.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

Hydroxylamine hydrochloride (21.40 g, 308 mmol) was added to a suspension of 1-(4-cyanophenyl)-3-dimethylaminopropen-1-one (55.96 g, 280 mmol) in MeOH (450 ml) and the reaction stirred at room temperature for 24 h. The reaction was diluted with water (400 ml) and the resultant precipitate collected by filtration, washed with water (5×150 ml) and dried in vacuo to give 4-(5-isoxazolyl)-benzonitrile as a pale yellow solid (42.53 g) m.p. 148-149°. δH (CDCl3) 8.35 (1H, d, J 1.8 Hz), 7.91 (2H, d, J 8.3 Hz), 7.77, (2H, d, J 8.3 Hz), 6.66 (1H, d, J 1.8 Hz).

後処理

  1. filtrationthe resultant precipitate collected by filtration
  2. washwashed with water (5×150 ml)
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-e0bfba8e587149d98e74c6fc92d98298
出典データセット
uspto-grants-2003_06
特許番号
US06579983B1

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