3-Aminophenol → 1-(3-Hydroxyanilino)-4-(4-pyridylmethyl)phthalazine

HRID 49868

반응식

HRID 49868 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([CH2:12][C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[N:4][N:3]=1.[NH2:19][C:20]1[CH:21]=[C:22]([OH:26])[CH:23]=[CH:24][CH:25]=1>C([O-])(=O)C.C(=O)([O-])[O-].[K+].[K+].CO>[OH:26][C:22]1[CH:21]=[C:20]([CH:25]=[CH:24][CH:23]=1)[NH:19][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([CH2:12][C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[N:4][N:3]=1

참가 물질

6

반응물 2

HCID 115683-AminophenolHCID 19446091-Chloro-4-(4-pyridinylmethyl)phthalazine

생성물 1

HCID 64193911-(3-Hydroxyanilino)-4-(4-pyridylmethyl)phthalazine

시약·촉매·용매 3

HCID 175Acetate용매HCID 887Methanol용매HCID 11430Potassium Carbonate용매

반응 조건

온도
120 °C

실험 절차

A mixture of 0.384 g (1.5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.491 g (4.5 mmol) 3-aminophenol is heated under nitrogen atmosphere for 1 h at 90° C. and for 3 h at 120° C. The reaction mixture is then taken up in a mixture of 30 ml acetate and 20 ml 20% aqueous potassium carbonate solution while stirring for about 4 h, and the filtration material is digested for 20 min in 20 ml of boiling methanol. After cooling to RT, filtration, washing of the filter residue with methanol, and drying under HV (8 h, 130° C.), title compound is obtained with a water content of 1.94%; m.p. 217-219° C.; ESI-MS: (M+H)+=329.

후처리

  1. temperatureAfter cooling to RT
  2. filtrationfiltration
  3. washwashing of the filter residue with methanol
  4. customdrying under HV (8 h, 130° C.)

출처 및 근거

ORD 기록
ord-13dac9bc62b74569911d6cec94e6ece0
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710047B2

연결된 노트

불러오는 중…