HCID 68585893、化合物 → 7-fluoro-5-methyl-2-[methyl(1H-1,2,4-triazol-5-ylmethyl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrile

HRID 17433ノート

反応式

HRID 17433 の反応式
[F:1][C:2]1[C:3]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[C:4]([CH3:30])[C:5]([C:28]#[N:29])=[C:6]2[C:10]=1[O:9][C:8]([N:11]([CH3:27])[CH2:12][C:13]1[N:14](CC3C=CC(OC)=CC=3)[N:15]=[CH:16][N:17]=1)=[N:7]2>FC(F)(F)C(O)=O>[F:1][C:2]1[C:3]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[C:4]([CH3:30])[C:5]([C:28]#[N:29])=[C:6]2[C:10]=1[O:9][C:8]([N:11]([CH3:27])[CH2:12][C:13]1[NH:14][N:15]=[CH:16][N:17]=1)=[N:7]2

参加物

3

反応物 1

HCID 68585893HCID 68585893、化合物

生成物 1

HCID 685848557-fluoro-5-methyl-2-[methyl(1H-1,2,4-triazol-5-ylmethyl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrile収率 97.4%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

7-Fluoro-2-[N-[[2-(4-methoxybenzyl)-2-H-[1,2,4]triazol-3-yl]methyl]methylamino]-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-164) (0.33 g, 0.68 mmol) was dissolved in trifluoroacetic acid (5 ml), and stirred at room temperature for 16 hours, then at an external temperature of about 60° C. for 6 hours. The solvent was evaporated away under reduced pressure, then ethyl acetate and aqueous sodium hydrogencarbonate solution were added, and the organic layer was separated. After drying over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=20:1) to obtain a colorless solid (0.24 g, 97%).

後処理

  1. waitat an external temperature of about 60° C. for 6 hours
  2. customThe solvent was evaporated away under reduced pressure
  3. additionethyl acetate and aqueous sodium hydrogencarbonate solution were added
  4. customthe organic layer was separated
  5. dry with materialAfter drying over anhydrous sodium sulfate
  6. customthe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=20:1)

出典と根拠

ORDレコード
ord-63d3818bb09c4d659eede15646fa4e51
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

反応ノート

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