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Potassium Nitrate → HCID 23358998, 화합물

HRID 232649
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HRID 232649 반응식
[F:1][C:2]1[C:7]([F:8])=[C:6]([CH3:9])[C:5]([F:10])=[CH:4][C:3]=1[CH3:11].[N+:12]([O-])([O-:14])=[O:13].[K+]>S(=O)(=O)(O)O>[F:8][C:7]1[C:2]([F:1])=[C:3]([CH3:11])[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([F:10])[C:6]=1[CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24434Potassium NitrateHCID 14651251HCID 14651251, 화합물

생성물 1

HCID 23358998HCID 23358998, 화합물수율 78.1%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

To 2,3,5-trifluoro-4-methyltoluene (1.9 g) is added conc. sulfuric acid (19 ml) and the mixture is cooled to 0° C., to which a solution of potassium nitrate (1.71 g) in conc. sulfuric acid (4.6 ml) is added dropwise below 10° C. and the mixture is stirred for 15 minutes. The 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 residue is purified by silica-gel column-chromatography (dichloro-methane: n-hexane=1:6) to give 2,3,6-trifluoro-4-methyl-5-nitrotoluene (1.9 g).

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후처리

  1. additionis added dropwise below 10° C.
  2. extractionextracted with diethyl ether
  3. washthe extract is washed with water
  4. customdried
  5. distillationThe solvent is distilled off under reduced pressure
  6. customthe residue is purified by silica-gel column-chromatography (dichloro-methane: n-hexane=1:6)

출처 및 근거

ORD 기록
ord-a2722392edeb4d0180fdef8f174eabf9
출처 데이터셋
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05591744

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