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Tert-Butyl nitrite → HCID 23359008, 화합물

HRID 2396958
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HRID 2396958 반응식
N(OC(C)(C)C)=O.[F:8][C:9]1[C:15]([CH3:16])=[C:14]([F:17])[C:13]([F:18])=[C:12]([N+:19]([O-:21])=[O:20])[C:10]=1N>CN(C)C=O>[F:17][C:14]1[C:13]([F:18])=[C:12]([N+:19]([O-:21])=[O:20])[CH:10]=[C:9]([F:8])[C:15]=1[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10906Tert-Butyl nitriteHCID 23359009HCID 23359009, 화합물

생성물 1

HCID 23359008HCID 23359008, 화합물수율 36.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of t-butyl nitrite (1.87 g) in anhydrous dimethylformamide (10.9 ml) is added dropwise a solution of 2,4,5-trifluoro-3-methyl-6-nitroaniline (2.05 g) in anhydrous dimethylformamide (16.4 ml) with stirring at 50°-52° C. and the mixture is stirred at the same temperature for 30 minutes. After cooling, the reaction mixture is poured into ice-water, extracted with diethyl ether, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the obtained residue is purified by silica-gel column-chromatography (eluent; dichloromethane : n-hexane=1 : 4) to give 2,3,6-trifluoro-4-nitrotoluene (0.7 g).

후처리

  1. stirringthe mixture is stirred at the same temperature for 30 minutes
  2. temperatureAfter cooling
  3. extractionextracted with diethyl ether
  4. washthe extract is washed with water
  5. customdried
  6. distillationThe solvent is distilled off under reduced pressure
  7. customthe obtained residue is purified by silica-gel column-chromatography (eluent; dichloromethane : n-hexane=1 : 4)

출처 및 근거

ORD 기록
ord-9c82d4eb3685460193548010532e55f7
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05495020

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