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Dimethylformamide → HCID 178428098, 화합물

HRID 471456
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HRID 471456 반응식
[Br:1][C:2]1[C:9]([CH3:10])=[CH:8][C:5](C#N)=[CH:4][C:3]=1[CH3:11].[N-:12]=[N+:13]=[N-:14].[Na+].[Cl-].[NH4+].[CH3:18][N:19](C)C=O>O>[Br:1][C:2]1[C:3]([CH3:11])=[CH:4][C:5]([N:13]2[N:14]=[CH:18][NH:19][NH:12]2)=[CH:8][C:9]=1[CH3:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 110850704-Bromo-3,5-dimethyl-benzonitrile

생성물 1

HCID 178428098HCID 178428098, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

4-Bromo-3,5-dimethyl benzonitrile (3.0 g, 14.3 mmol), sodium azide (2.32 g, 35.7 mmol) and ammonium chloride (2.3 g, 42.84 mmol) are suspended in dry N,N-dimethylformamide and heated at 140° C. for 7 hours. The mixture is allowed to cool to room temperature, diluted with water and the precipitated solid collected by filtration, washed with water and dried to give the title compound (yield 1.74 g). The mother liquor was saturated with sodium chloride and repeatedly extracted with ethyl acetate. The organic extracts were combined and the solvent removed to give a second crop of title compound (yield 1.39 g, total yield 3.13 g).

후처리

  1. temperatureto cool to room temperature
  2. filtrationthe precipitated solid collected by filtration
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-0895e80ecd6043b5802516dc1cf69599
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08633182B2

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