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

HRID 376536

반응식

HRID 376536 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6695f32bf3964c77b3ffb225e94d8322
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06020334

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