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Trifluoroacetic acid → 4-(1-(3,5-dimethyl-1H-pyrazol-1-yl)ethyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-amine

HRID 1930713
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반응식

HRID 1930713 반응식
[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([CH:8]([C:10]2[C:11]3[CH2:34][N:33](C(OC(C)(C)C)=O)[CH2:32][CH2:31][C:12]=3[N:13]=[C:14]([NH:16][C:17]3[CH:22]=[CH:21][C:20]([N:23]4[CH:27]=[C:26]([CH3:28])[N:25]=[CH:24]4)=[C:19]([O:29][CH3:30])[CH:18]=3)[N:15]=2)[CH3:9])[N:3]=1.C(O)(C(F)(F)F)=O.C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([CH:8]([C:10]2[C:11]3[CH2:34][NH:33][CH2:32][CH2:31][C:12]=3[N:13]=[C:14]([NH:16][C:17]3[CH:22]=[CH:21][C:20]([N:23]4[CH:27]=[C:26]([CH3:28])[N:25]=[CH:24]4)=[C:19]([O:29][CH3:30])[CH:18]=3)[N:15]=2)[CH3:9])[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 59333720HCID 59333720, 화합물

생성물 1

HCID 593337574-(1-(3,5-dimethyl-1H-pyrazol-1-yl)ethyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-amine수율 77%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

A solution of tert-butyl 4-(1-(3,5-dimethyl-1H-pyrazol-1-yl)ethyl)-2-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenylamino)-7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate (397 mg, 0.71 mmol) and TFA (0.547 mL, 7.10 mmol) in DCM was stirred for one hour at 40° C. The reaction mixture was cooled and sat aqu NaHCO3 was added until the mixture was neutralized. The organic phase was separated and the water phase was washed repeatedly with DCM yielding 4-(1-(3,5-dimethyl-1H-pyrazol-1-yl)ethyl)-N-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-2-amine (250 mg, 77%)

후처리

  1. temperatureThe reaction mixture was cooled
  2. additionwas added until the mixture
  3. customThe organic phase was separated
  4. washthe water phase was washed repeatedly with DCM

출처 및 근거

ORD 기록
ord-0d45801f58374ca899b67bdb19bf4e6f
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188101B2

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