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Dimethylformamide → 2-(2-Azido-1-ethoxyethylideneamino)-5-nitrobenzophenone

HRID 867060
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HRID 867060 반응식
Br[CH2:2][C:3](=[N:7][C:8]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][C:9]=1[C:10]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:11])[O:4][CH2:5][CH3:6].CN(C)C=O.[N-:30]=[N+:31]=[N-:32].[Na+].C(OCC)(=O)C>O>[N:30]([CH2:2][C:3](=[N:7][C:8]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][C:9]=1[C:10]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:11])[O:4][CH2:5][CH3:6])=[N+:31]=[N-:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 33557Sodium AzideHCID 203172702-(2-Bromo-1-ethoxyethylideneamino)-5-nitrobenzophenone

생성물 1

HCID 203172632-(2-Azido-1-ethoxyethylideneamino)-5-nitrobenzophenone

시약·촉매·용매 1

HCID 962Water
용매

실험 절차

To a solution of 3.3 parts of 2-(2-bromo-1-ethoxyethylideneamino)-5-nitrobenzophenone produced in Step (1) in 15 parts by volume of dimethylformamide is added 0.5 part of sodium azide at a room temperature with stirring. After the stirring is continued for further 40 minutes. Ethyl acetate and water are added to the reaction mixture and shaken well. The ethyl acetate layer separated is washed with water and dried over anhydrous sodium sulfate. Evaporation of the solvent gives 2-(2-azido-1-ethoxyethylideneamino)-5-nitrobenzophenone as an oily substance. The product shows an absorption band at 2077 cm-1 due to N3 in an infrared absorption spectrum.

후처리

  1. stirringshaken well
  2. customThe ethyl acetate layer separated
  3. washis washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-0babb624e4964314aa8ad455c735fed5
출처 데이터셋
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04102881

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