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Phosphorus trichloride → HCID 501246, 화합물

HRID 2300998
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HRID 2300998 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[CH:9]([S:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N+:15]=1[O-])(=[O:13])=[O:12])[CH3:10].P(Cl)(Cl)Cl>C(Cl)(Cl)Cl>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[CH:9]([S:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1)(=[O:12])=[O:13])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24387Phosphorus trichlorideHCID 501133Dimenoxypyrin

생성물 1

HCID 501246HCID 501246, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 4.7 g (0.017 mole) of 2-[1-(2,5-Dimethylphenyl)-ethylsulfonyl]-pyridine-N-oxide, 60 ml of chloroform, and 7.5 g (0.055 mole) of PCl3 were placed in a 100 ml round bottom flask equipped with a magnetic stirrer and reflux condenser. The mixture was refluxed for one hour, and then the solvent was removed under reduced pressure using a rotovap. To the residue was added 25 ml of ethanol, followed by a second evaporation. The residue crystallized to give a white solid, which was recrystallized from ethanol. Obtained were 3.0 g of product having a melting point of 95-96° C. The IR, NMR and mass spectra were consistent with the proposed structure.

후처리

  1. customwere placed in a 100 ml round bottom flask
  2. customequipped with a magnetic stirrer
  3. temperaturereflux condenser
  4. temperatureThe mixture was refluxed for one hour
  5. customthe solvent was removed under reduced pressure
  6. additionTo the residue was added 25 ml of ethanol
  7. customfollowed by a second evaporation
  8. customThe residue crystallized
  9. customto give a white solid, which
  10. customwas recrystallized from ethanol
  11. customObtained

출처 및 근거

ORD 기록
ord-c96ba3c5839742578ac2fde5cebb90f3
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06498254B1

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