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

HRID 49887

반응식

HRID 49887 반응식
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

참가 물질

3

반응물 2

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

생성물 1

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

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bfebeffd30d7440f9ff39ed3b4d13f36
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710047B2

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