Potassium Carbonate → HCID 71515487, 화합물

HRID 1466214노트

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HRID 1466214 반응식
[F:1][C:2]([F:37])([F:36])[C:3]1[CH:4]=[C:5]([CH:29]=[C:30]([C:32]([F:35])([F:34])[F:33])[CH:31]=1)[CH2:6][NH:7][CH2:8][C:9]1[CH:10]=[C:11]2[C:26]([CH3:27])=[N:25][N:24]([CH3:28])[C:12]2=[N:13][C:14]=1[N:15]([CH2:20][CH:21]1[CH2:23][CH2:22]1)[CH2:16][CH:17]1[CH2:19][CH2:18]1.Cl[C:39]1[N:44]=[CH:43][C:42]([C:45](=[O:47])[CH3:46])=[CH:41][N:40]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH:17]1([CH2:16][N:15]([CH2:20][CH:21]2[CH2:23][CH2:22]2)[C:14]2[N:13]=[C:12]3[N:24]([CH3:28])[N:25]=[C:26]([CH3:27])[C:11]3=[CH:10][C:9]=2[CH2:8][N:7]([CH2:6][C:5]2[CH:29]=[C:30]([C:32]([F:34])([F:35])[F:33])[CH:31]=[C:3]([C:2]([F:36])([F:1])[F:37])[CH:4]=2)[C:39]2[N:44]=[CH:43][C:42]([C:45](=[O:47])[CH3:46])=[CH:41][N:40]=2)[CH2:18][CH2:19]1

참가 물질

5

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HCID 11430Potassium CarbonateHCID 137157421-(2-Chloropyrimidin-5-yl)ethan-1-oneHCID 894804125-(((3,5-bis(trifluoromethyl)benzyl)amino)methyl)-N,N-bis(cyclopropylmethyl)-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridin-6-amine

생성물 1

HCID 71515487HCID 71515487, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
65 °C

실험 절차

5-(((3,5-bis(trifluoromethyl)benzyl)amino)methyl)-N,N-bis(cyclopropylmethyl)-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridin-6-amine (0.761 mmol, 0.400 g) in DMF was treated with 1-(2-chloropyrimidin-5-yl)ethanone (0.761 mmol, 0.119 g) and K2CO3 (2.283 mmol, 0.315 g). The reaction mixture was stirred at 60-70° C. for 12-16 h. The reaction mixture was then extracted with EtOAc. The combined organic layer was washed with water and brine solution, dried over sodium sulphate, concentrated under reduced pressure and purified by column chromatography using silica gel and 50% EtOAc in petroleum ether as eluent to get the title compound.

후처리

  1. extractionThe reaction mixture was then extracted with EtOAc
  2. washThe combined organic layer was washed with water and brine solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated under reduced pressure
  5. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-d53933d784e443bfad8d35c5125edda2
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09000007B2

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