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

HRID 49868

反応式

HRID 49868 の反応式
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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 175Acetate溶媒HCID 887Methanol溶媒HCID 11430Potassium Carbonate溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-13dac9bc62b74569911d6cec94e6ece0
出典データセット
uspto-grants-2004_03
特許番号
US06710047B2

関連ノート

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