Water → 3-(3-bromo-phenyl)-6-chloro-1-trityl-1H-pyrazolo[3,4-d]pyrimidine

HRID 1809710노트

반응식

HRID 1809710 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:8]2[C:16]3[C:11](=[N:12][C:13]([Cl:17])=[N:14][CH:15]=3)[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.CCN(CC)CC.[C:25](Cl)([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.O>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]([C:8]2[C:16]3[C:11](=[N:12][C:13]([Cl:17])=[N:14][CH:15]=3)[N:10]([C:25]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)([C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=3)[C:32]3[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=3)[N:9]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 178478326HCID 178478326, 화합물

생성물 1

HCID 866679653-(3-bromo-phenyl)-6-chloro-1-trityl-1H-pyrazolo[3,4-d]pyrimidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a mixture of 3-(3-bromo-phenyl)-6-chloro-1H-pyrazolo[3,4-d]pyrimidine (from Example 38 supra) (4.0 g, 12.9 mmol) and Et3N (2.6 g, 25.8 mmol) in DMF (40 mL) was added the solution of trityl chloride (4.3 g, 15.5 mmol) in DMF (40 mL) at room temperature. This mixture was stirred at room temperature for 2 hours. The reaction solution was then poured into water (400 mL), and the yellow precipitate was collected by filtration. This crude product was purified by chromatography (silica gel, dichloromethane:petroleum ether, 1:1) to give 3-(3-bromo-phenyl)-6-chloro-1-trityl-1H-pyrazolo[3,4-d]pyrimidine as a light yellow solid. (Yield 3.5 g, 30%).

후처리

  1. filtrationthe yellow precipitate was collected by filtration
  2. customThis crude product was purified by chromatography (silica gel, dichloromethane:petroleum ether, 1:1)

출처 및 근거

ORD 기록
ord-424b570a0cd54ebdb5f740742d04594a
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362023B2

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