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2-Amino-5-nitrobenzophenone → 4-Phenyl-6-nitro-quinazoline

HRID 919176
노트
인쇄 미리보기

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HRID 919176 반응식
[NH2:1][C:2]1[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=O.[NH2:19][C:20](N)=S>CS(C)=O>[C:6]1([C:4]2[C:3]3[C:2](=[CH:15][CH:14]=[C:13]([N+:16]([O-:18])=[O:17])[CH:12]=3)[N:1]=[CH:20][N:19]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 156812-Amino-5-nitrobenzophenoneHCID 2723790Thiourea

생성물 1

HCID 142028674-Phenyl-6-nitro-quinazoline수율 39.7%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
140 °C

실험 절차

To a 20 mL microwave reaction vial with a micro magnetic stir bar, were added 0.297 g of 2-amino-5-nitrobenzophenone, 0.186 g of thiourea and 3.0 mL of DMSO. Then the vial was sealed and heated with microwave at 140° C. for 20 hours. Two layers of liquid formed with brown liquid on the top and a dark brown gel like layer at the bottom. The reaction mixture was extracted with EtOAc and purified on column chromatography using hexane/EtOAc (5:1 to 4:1) as eluent, and 0.122 g of 4-phenyl-6-nitro-quinazoline was obtained, in a yield of 39.7%.

후처리

  1. customTo a 20 mL microwave reaction vial with a micro magnetic stir bar
  2. customThen the vial was sealed
  3. customTwo layers of liquid formed with brown liquid on the top
  4. extractionThe reaction mixture was extracted with EtOAc
  5. custompurified on column chromatography

출처 및 근거

ORD 기록
ord-59ddccb812964018a0a9e81210fdb4bd
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273012B2

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