Nitric Acid → Quintozene

HRID 1462968

반응식

HRID 1462968 반응식
[Cl:1][C:2]1[C:7](S)=[C:6]([Cl:9])[C:5]([Cl:10])=[C:4]([Cl:11])[C:3]=1[Cl:12].[N+:13]([O-])([OH:15])=[O:14].ClC1C(Cl)=C(Cl)C(Cl)=C(Cl)C=1Cl>OS(O)(=O)=O.O=S(=O)=O>[C:7]1([N+:13]([O-:15])=[O:14])[C:2]([Cl:1])=[C:3]([Cl:12])[C:4]([Cl:11])=[C:5]([Cl:10])[C:6]=1[Cl:9]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 8370HexachlorobenzeneHCID 8620Pentachlorothiophenol

생성물 1

HCID 6720Quintozene수율 74%

시약·촉매·용매 1

HCID 24681Fuming sulfuric acid용매

실험 절차

Pentachlorothiophenol (10.0 g, 0.035 mol) was added to 60.0 g of 70% nitric acid at room temperature. The reaction mixture was heated at reflux 7 hr followed by stirring at room temperature 16 hr. At this point, 40 mL of 30% oleum (30% by weight sulfur trioxide in sulfuric acid) was added at such a rate that the temperature was maintained between 55° and 60° C. After the addition was complete (30 min), the reaction mixture was heated at 108° C. for 30 minutes. The reaction mixture was then cooled to room temperature, filtered, the product washed with water and dried in vacuo to give 7.6 g (74% yield) of 99.0% PCNB with 1.0% hexachlorobenzene (GC assay).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux 7 hr
  3. temperaturewas maintained between 55° and 60° C
  4. additionAfter the addition
  5. custom(30 min)
  6. temperaturethe reaction mixture was heated at 108° C. for 30 minutes
  7. temperatureThe reaction mixture was then cooled to room temperature
  8. filtrationfiltered
  9. washthe product washed with water
  10. customdried in vacuo

출처 및 근거

ORD 기록
ord-4362a6675632469e9c100365aadfbaac
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04461918

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