Benzenamine, 3-chloro-, hydrochloride (1:1) → 3-[2-(Boc-amino)-ethylamino]-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine

HRID 1068956

反応式

HRID 1068956 の反応式
[C:1]([NH:8][CH2:9][CH2:10][NH:11][C:12]1[C:16]([C:17]#[N:18])=[C:15]([N:19]([CH3:21])C)[N:14](N=C)[N:13]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].Cl.[Cl:25][C:26]1[CH:27]=[C:28]([CH:30]=[CH:31][CH:32]=1)[NH2:29]>CO>[C:4]([O:3][C:1]([NH:8][CH2:9][CH2:10][NH:11][C:12]1[C:16]2[C:15](=[N:19][CH:21]=[N:18][C:17]=2[NH:29][C:28]2[CH:30]=[CH:31][CH:32]=[C:26]([Cl:25])[CH:27]=2)[NH:14][N:13]=1)=[O:2])([CH3:7])([CH3:6])[CH3:5]

参加物

4

反応物 2

HCID 67336Benzenamine, 3-chloro-, hydrochloride (1:1)HCID 696975253-[2-(Boc-amino)-ethylamino]-4-cyano-5-dimethylamino-methyleneamino-pyrazole

生成物 1

HCID 211906093-[2-(Boc-amino)-ethylamino]-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 35 g (108.9 mmol) of 3-[2-(Boc-amino)-ethylamino]-4-cyano-5-dimethylamino-methyleneamino-pyrazole, 17.9 g (109.1 mmol) of 3-chloro-aniline hydrochloride and 350 ml of methanol is heated under reflux for 30 hours and then stirred at RT for 15 hours. Filtration and washing the filter residue with methanol yield 3-[2-(tert-butyloxy-carbonyl-amino)-ethylamino]-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine having a water content of 2.39%; m.p. 206-208° C.; ESI-MS: (M−H)−=402.

後処理

  1. temperatureis heated
  2. temperatureunder reflux for 30 hours
  3. filtrationFiltration
  4. washwashing the filter residue with methanol

出典と根拠

ORDレコード
ord-42c25ec23f3a40fdb1defd6213fbaf90
出典データセット
uspto-grants-2001_06
特許番号
US06251911B1

関連ノート

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