4-Pyridinemethanamine → 1-(4-Chloroanilino)-4-(4-pyridylmethylamino)phthalazine

HRID 1384128

反応式

HRID 1384128 の反応式
Cl.Cl[C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([NH:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[N:5][N:4]=1.[NH2:21][CH2:22][C:23]1[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=1>>[Cl:20][C:17]1[CH:18]=[CH:19][C:14]([NH:13][C:6]2[C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[C:3]([NH:21][CH2:22][C:23]3[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=3)=[N:4][N:5]=2)=[CH:15][CH:16]=1

参加物

3

反応物 2

HCID 773174-PyridinemethanamineHCID 223972781-Chloro-4-(4-chloroanilino)phthalazine hydrochloride

生成物 1

HCID 63264211-(4-Chloroanilino)-4-(4-pyridylmethylamino)phthalazine

反応条件

温度
90 °C

実験手順

A mixture of 0.5 g (1.5436 mmol) 1-chloro-4-(4-chloroanilino)phthalazine hydrochloride (for preparation see J. Chem. Soc. 1948, 777-782) and 2 g (18.50 mmol) 4-aminomethylpyridine is stirred for 36 h at 90° C. and then purified by means of flash chromatography on silica gel with a particle size of 0.04-0.06 mm using acetate and acetate/methanol (20:1). Evaporation of product-containing fractions, recrystallization of the residue from methanol, and drying of the crystallizate under HV yield the title compound; m.p. 233-236° C.; ESI-MS: (M+H)+=362.

後処理

  1. custompurified by means of flash chromatography on silica gel with a particle size of 0.04-0.06 mm
  2. customEvaporation of product-containing fractions, recrystallization of the residue from methanol
  3. customdrying of the crystallizate under HV

出典と根拠

ORDレコード
ord-407c115576a04ffd9adb4e26340f4ae3
出典データセット
uspto-grants-2001_07
特許番号
US06258812B1

関連ノート

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