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Dimethylacetamide → HCID 59129370, 화합물

HRID 1847818
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HRID 1847818 반응식
[C:1]([C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][C:6]=1[N+:15]([O-:17])=[O:16])([CH3:4])([CH3:3])[CH3:2].C(C1C=CC([N+]([O-])=O)=C(C)C=1[N+]([O-])=O)(C)(C)C.C[C:36]([N:38]([CH3:40])[CH3:39])=O>CN(C=O)C>[C:1]([C:5]1[C:6]([N+:15]([O-:17])=[O:16])=[CH:7][C:8]([N+:12]([O-:14])=[O:13])=[C:9](/[CH:11]=[CH:36]/[N:38]([CH3:40])[CH3:39])[CH:10]=1)([CH3:4])([CH3:2])[CH3:3]
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참가 물질

5

반응물 3

HCID 31374DimethylacetamideHCID 533645731-Tert-butyl-5-methyl-2,4-dinitrobenzeneHCID 591294471-Tert-butyl-3-methyl-2,4-dinitrobenzene

생성물 1

HCID 59129370HCID 59129370, 화합물수율 68%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1-tert-butyl-5-methyl-2,4-dinitrobenzene and 1-tert-butyl-3-methyl-2,4-dinitrobenzene (9.0 g, 38 mmol, 2:1 by NMR) and DMA (5.4 g, 45 mmol) in DMF (50 mL) was heated at reflux for 2 h before being cooled to room temperature. The reaction mixture was poured into water-ice and extracted with EtOAc (50 mL×3). The combined organic layers were washed with water and brine, before being evaporated to give a brown oil, which was purified by column to give (E)-2-(5-tert-butyl-2,4-dinitrophenyl)-N,N-dimethylethen-amine (5.0 g, 68%).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 h
  3. extractionextracted with EtOAc (50 mL×3)
  4. washThe combined organic layers were washed with water and brine
  5. custombefore being evaporated
  6. customto give a brown oil, which
  7. customwas purified by column

출처 및 근거

ORD 기록
ord-2f16bc5509964fd78078af437e473b26
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952049B2

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