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

反応式

HRID 59142 の反応式
[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]

参加物

5

反応物 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

生成物 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)ethanol収率 10.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-3f2d214a44524b1da474bd00f531e764
出典データセット
uspto-grants-2016_09
特許番号
US09439904B2

関連ノート

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