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2-amino-N-(4-chlorophenyl)benzamide → HCID 67455493, 화합물

HRID 1846362
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HRID 1846362 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11])[CH:5]=O.[NH2:13][C:14]1[CH:29]=[CH:28][CH:27]=[CH:26][C:15]=1[C:16]([NH:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)=[O:17]>CCO>[Cl:25][C:22]1[CH:23]=[CH:24][C:19]([N:18]2[C:16](=[O:17])[C:15]3[C:14](=[CH:29][CH:28]=[CH:27][CH:26]=3)[N:13]=[C:5]2[C:4]2[CH:7]=[CH:8][C:9]([N+:10]([O-:12])=[O:11])=[C:2]([CH3:1])[CH:3]=2)=[CH:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6704722-amino-N-(4-chlorophenyl)benzamideHCID 111945283-Methyl-4-nitrobenzaldehyde

생성물 1

HCID 67455493HCID 67455493, 화합물수율 48%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3-methyl-4-nitro-benzaldehyde (0.268 g, 1.60 mmol) and anyhydrous CuCl2 (0.437 g, 3.20 mmol) were added to a solution of 2-amino-N-(4-chlorophenyl)benzamide (0.400 g, 1.60 mmol) in anyhydrous EtOH (15 mL) and heated at reflux temperature for 3.5 hours. After concentration in vacuo and dissolving the residue in EtOAc, the organics were washed with H2O, then brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash chromatography on silica gel, eluting with 10% to 70% EtOAc in heptane, afforded 3-(4-chlorophenyl)-2-(3-methyl-4-nitrophenyl)quinazolin-4(3H)-one (0.300 g, 48%).

후처리

  1. temperatureheated
  2. temperatureat reflux temperature for 3.5 hours
  3. concentrationAfter concentration in vacuo
  4. dissolutiondissolving the residue in EtOAc
  5. washthe organics were washed with H2O
  6. dry with materialbrine, dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customPurification by flash chromatography on silica gel
  10. washeluting with 10% to 70% EtOAc in heptane

출처 및 근거

ORD 기록
ord-dfef2c3f5ede4a928c78a1f7dcb42de2
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952021B2

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