Potassium Carbonate → 2,2,2-Trifluoro-1-(2-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenylamino)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-yl)ethanol

HRID 59142

반응식

HRID 59142 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:15][C:16]2[N:21]=[C:20]([CH:22]=[O:23])[CH:19]=[C:18]([CH2:24][O:25][CH2:26][C:27]([F:30])([F:29])[F:28])[N:17]=2)[CH:6]=[CH:7][C:8]=1[N:9]1[CH:13]=[C:12]([CH3:14])[N:11]=[CH:10]1.C(=O)([O-])[O-].[K+].[K+].[F:37][C:38]([Si](C)(C)C)([F:40])[F:39]>CN(C=O)C>[F:37][C:38]([F:40])([F:39])[CH:22]([C:20]1[CH:19]=[C:18]([CH2:24][O:25][CH2:26][C:27]([F:29])([F:30])[F:28])[N:17]=[C:16]([NH:15][C:5]2[CH:6]=[CH:7][C:8]([N:9]3[CH:13]=[C:12]([CH3:14])[N:11]=[CH:10]3)=[C:3]([O:2][CH3:1])[CH:4]=2)[N:21]=1)[OH:23]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 552549(Trifluoromethyl)trimethylsilaneHCID 1178240362-(3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)phenylamino)-6-((2,2,2-trifluoroethoxy)methyl)-pyrimidine-4-carbaldehyde

생성물 1

HCID 863440702,2,2-Trifluoro-1-(2-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenylamino)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-yl)ethanol수율 10.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Molecular sieves were added to a solution of 2-(3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenylamino)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine-4-carbaldehyde (60 mg, 0.14 mmol) in dry DMF (1 mL) under argon atmosphere. The mixture was stirred for 30 minutes. Potassium carbonate (2 mg, 0.01 mmol) and (trifluoromethyl)trimethylsilane (0.427 mL, 0.21 mmol) were added. The mixture was stirred at ambient temperature for 2 days. The mixture was filtered and purified by preparative HPLC to yield the title compound (7 mg, 10%).

후처리

  1. stirringThe mixture was stirred at ambient temperature for 2 days
  2. filtrationThe mixture was filtered
  3. custompurified by preparative HPLC

출처 및 근거

ORD 기록
ord-3f2d214a44524b1da474bd00f531e764
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09439904B2

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