3-(4-sec-butylphenyl)-2-(3,4-dinitrophenyl)quinazolin-4(3H)-one → 3-(4-sec-butylphenyl)-2-(3,4-diaminophenyl)quinazolin-4(3H)-one

HRID 1846366ノート

反応式

HRID 1846366 の反応式
[CH:1]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:20](=[O:21])[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[N:13]=[C:12]2[C:22]2[CH:27]=[CH:26][C:25]([N+:28]([O-])=O)=[C:24]([N+:31]([O-])=O)[CH:23]=2)=[CH:7][CH:6]=1)([CH2:3][CH3:4])[CH3:2]>CCO>[CH:1]([C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C:20](=[O:21])[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[N:13]=[C:12]2[C:22]2[CH:27]=[CH:26][C:25]([NH2:28])=[C:24]([NH2:31])[CH:23]=2)=[CH:9][CH:10]=1)([CH2:3][CH3:4])[CH3:2]

参加物

3

反応物 1

HCID 866598193-(4-sec-butylphenyl)-2-(3,4-dinitrophenyl)quinazolin-4(3H)-one

生成物 1

HCID 866598203-(4-sec-butylphenyl)-2-(3,4-diaminophenyl)quinazolin-4(3H)-one収率 62.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3-(4-sec-butylphenyl)-2-(3,4-dinitrophenyl)quinazolin-4(3H)-one (0.240 g, 0.54 mmol) was dissolved in EtOH (20 mL) and flushed with N2 for 15 minutes. Pd/C (0.025 g, 10 wt %) was added, and stirred under 1 atmosphere of H2 overnight. After flushing with N2, the mixture was filtered through diatomaceous earth. The filtrate was concentrated and purified by flash chromatography on silica gel, eluting with 0% to 10% MeOH in EtOAc, to afford 3-(4-sec-butylphenyl)-2-(3,4-diaminophenyl)quinazolin-4(3H)-one (0.130 g, 62%).

後処理

  1. customflushed with N2 for 15 minutes
  2. additionPd/C (0.025 g, 10 wt %) was added
  3. customAfter flushing with N2
  4. filtrationthe mixture was filtered through diatomaceous earth
  5. concentrationThe filtrate was concentrated
  6. custompurified by flash chromatography on silica gel
  7. washeluting with 0% to 10% MeOH in EtOAc

出典と根拠

ORDレコード
ord-77c01d0d43424793bc47aecf07e091a2
出典データセット
uspto-grants-2015_02
特許番号
US08952021B2

反応ノート

読み込み中…