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

반응식

HRID 520438 반응식
[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]

참가 물질

4

반응물 1

HCID 585528473-methyl-8-nitro-2-(3-(trifluoromethyl)phenyl)quinazolin-4(3H)-one

생성물 1

HCID 585528228-amino-3-methyl-2-(3-(trifluoromethyl)phenyl)quinazolin-4(3H)-one수율 93.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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%)

출처 및 근거

ORD 기록
ord-c7c3d3f51a474447b0c08cb58f1ddbdf
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09326986B2

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