Hydroxyamine hydrochloride → 4-(3-chlorophenyl)-1-ethyl-7-hydroxyiminomethylpyrido[2,3-d]pyrimidin-2(1H)-one

HRID 368992노트

반응식

HRID 368992 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:9]3[CH:20]=[CH:19][C:18]([CH:21]=O)=[N:17][C:10]=3[N:11]([CH2:15][CH3:16])[C:12](=[O:14])[N:13]=2)[CH:5]=[CH:6][CH:7]=1.Cl.[NH2:24][OH:25].C([O-])(=O)C.[Na+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[C:9]3[CH:20]=[CH:19][C:18]([CH:21]=[N:24][OH:25])=[N:17][C:10]=3[N:11]([CH2:15][CH3:16])[C:12](=[O:14])[N:13]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 23284478HCID 23284478, 화합물

생성물 1

HCID 1363337144-(3-chlorophenyl)-1-ethyl-7-hydroxyiminomethylpyrido[2,3-d]pyrimidin-2(1H)-one수율 18%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-(3-Chlorophenyl)-1-ethyl-2-oxo-1,2-dihydropyrido[2,3-d]pyrimidine-7-carbaldehyde (900 mg, 2.9 mmol) was dissolved in 10 ml of methanol, 420 mg (6.0 mmol) of hydroxylamine hydrochloride and 550 mg (6.7 mmol) of sodium acetate were added thereto, followed by stirring overnight at room temperature. The insoluble matter was washed with water and chloroform and recrystallized from dimethylformamide-acetonitrile to give 171 mg (18%) of 4-(3-chlorophenyl)-1-ethyl-7-hydroxyiminomethylpyrido[2,3-d]pyrimidin-2(1H)-one.

후처리

  1. washThe insoluble matter was washed with water and chloroform
  2. customrecrystallized from dimethylformamide-acetonitrile

출처 및 근거

ORD 기록
ord-4b06b3b2b3f447afb91b2642d2b0c61e
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06136810

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