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

HRID 1068956

반응식

HRID 1068956 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-42c25ec23f3a40fdb1defd6213fbaf90
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06251911B1

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