Sodium Sulfate → 4-(Pentafluorophenyl)-1,2,4-triazoline-3,5-dione

HRID 1902896

반응식

HRID 1902896 반응식
[F:1][C:2]1[C:7]([N:8]2[C:12](=[O:13])[NH:11][NH:10][C:9]2=[O:14])=[C:6]([F:15])[C:5]([F:16])=[C:4]([F:17])[C:3]=1[F:18].S([O-])([O-])(=O)=O.[Na+].[Na+]>C(OCC)(=O)C>[F:15][C:6]1[C:7]([N:8]2[C:9](=[O:14])[N:10]=[N:11][C:12]2=[O:13])=[C:2]([F:1])[C:3]([F:18])=[C:4]([F:17])[C:5]=1[F:16]

참가 물질

4

반응물 2

HCID 24436Sodium SulfateHCID 129043794-(Pentafluorophenyl)urazole

생성물 1

HCID 129043834-(Pentafluorophenyl)-1,2,4-triazoline-3,5-dione

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A 50 ml, three-necked flask is fitted with a gas-dispersion tube, a drying tube and a stirrer. 4-(Pentafluorophenyl)urazole, 0.5 g (1.8 mM) is dissolved in 25 ml of ethyl acetate. Anhydrous sodium sulfate, 3 g, is added to remove water present in NO2. The reaction mixture is cooled in an ice bath, and nitrogen dioxide added slowly for 20 minutes. The mixture is allowed to stir for 20 minutes. The Na2SO4 is removed by filtration and the ethyl acetate removed with the rotary evaporator to yield a red oil. The residual solvent is removed with a vacuum pump to yield a crystalline solid, 0.35 g, mp 88°-91° C. The product is further purified by sublimation, mp 94°-96° C.

후처리

  1. customA 50 ml, three-necked flask is fitted with a gas-dispersion tube, a drying tube and a stirrer
  2. customto remove water
  3. temperatureThe reaction mixture is cooled in an ice bath
  4. additionnitrogen dioxide added slowly for 20 minutes
  5. customThe Na2SO4 is removed by filtration
  6. customthe ethyl acetate removed with the rotary evaporator
  7. customto yield a red oil
  8. customThe residual solvent is removed with a vacuum pump
  9. customto yield a crystalline solid, 0.35 g, mp 88°-91° C
  10. customThe product is further purified by sublimation, mp 94°-96° C.

출처 및 근거

ORD 기록
ord-2b0fa37bf6af4c12bd1c9bb8c74e4ee2
출처 데이터셋
uspto-grants-1982_12
특허 번호
US04366320

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