Water → 4-(Amino-hydroxyimino)methylbenzoic acid methyl ester

HRID 376536

反応式

HRID 376536 の反応式
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[N:11])=[CH:6][CH:5]=1.Cl.[NH2:14][OH:15].C(=O)([O-])O.[Na+].O>CO>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([CH:10]=[N:11][O:15][NH2:14])=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 962WaterHCID 70791Methyl 4-cyanobenzoateHCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 543937604-(Amino-hydroxyimino)methylbenzoic acid methyl ester収率 81%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 200 ml of methanol were dissolved 16.5 g of 4-cyanobenzoic acid methyl ester and 7.2 g of hydroxylamine hydrochloride. To the solution was added 8.82 g of sodium hydrogencarbonate at room temperature. The mixture was heated for 3 hours under reflux. The reaction mixture was cooled, to which was added 400 ml of water. Resulting crystalline precipitate was collected by filtration, which was washed with water and ether, followed by drying under reduced pressure to afford 16.1 g of the titled compound as colorless needles.

後処理

  1. temperatureThe mixture was heated for 3 hours
  2. temperatureunder reflux
  3. temperatureThe reaction mixture was cooled, to which
  4. filtrationResulting crystalline precipitate was collected by filtration, which
  5. washwas washed with water and ether
  6. customby drying under reduced pressure

出典と根拠

ORDレコード
ord-6695f32bf3964c77b3ffb225e94d8322
出典データセット
uspto-grants-2000_02
特許番号
US06020334

関連ノート

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