3-methyl-8-nitro-2-(3-(trifluoromethyl)phenyl)quinazolin-4(3H)-one → 8-amino-3-methyl-2-(3-(trifluoromethyl)phenyl)quinazolin-4(3H)-one

HRID 520438

反応式

HRID 520438 の反応式
[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[C:5](=[C:6]([N+:13]([O-])=O)[CH:7]=[CH:8][CH:9]=2)[N:4]=[C:3]1[C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:17]=1>C1COCC1.[Pd]>[NH2:13][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[N:4]=[C:3]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:17]=1)[N:2]([CH3:1])[C:11]2=[O:12]

参加物

4

実験手順

Pd/C 10 wt % (100 mg) was added to a degassed solution of 3-methyl-8-nitro-2-(3-(trifluoromethyl)phenyl)quinazolin-4(3H)-one 4 (1.3 g, 3.7 mmol) in THF (35 mL). The mixture was hydrogenated under balloon pressure for 12 h. The catalyst was removed by filtration and the solvent evaporated. The residue was purified by MPLC eluting with pentane/EtOAc (0-50%) to give 5 (1.1 g, 90% yield) as a yellow solid.

後処理

  1. customThe catalyst was removed by filtration
  2. customthe solvent evaporated
  3. customThe residue was purified by MPLC
  4. washeluting with pentane/EtOAc (0-50%)

出典と根拠

ORDレコード
ord-c7c3d3f51a474447b0c08cb58f1ddbdf
出典データセット
uspto-grants-2016_05
特許番号
US09326986B2

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