Nitric Acid → Quintozene

HRID 1263034

反応式

HRID 1263034 の反応式
[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].OS(O)(=O)=O.O=S(=O)=O.ClC1C(Cl)=C(Cl)C(Cl)=C(Cl)C=1Cl>>[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]

参加物

5

反応物 4

HCID 944Nitric AcidHCID 8370HexachlorobenzeneHCID 8620PentachlorothiophenolHCID 24681Fuming sulfuric acid

生成物 1

HCID 6720Quintozene収率 85%

反応条件

温度
55 °C

実験手順

Pentachlorothiophenol (10.0 g, 0.035 mol) was added to 60.0 g of 99% nitric acid over 20 min at 45°-50° C. followed by heating at reflux (55° C.) for 1.5 hr. At this point 20 mL of 30% by weight oleum was added at such a rate that the temperature was kept at 75° to 80° C. After the addition was complete (approximately 30 min.), the reaction mixture was cooled to room temperature. The product was collected by filtration, and thoroughly washed with water to give after drying in vacuo, 8.6 g (85% yield) of 99.7% PCNB with 0.17% hexachlorobenzene (GC assay). Variations on this one-pot, two-step process were examined and are summarized in TABLE I.

後処理

  1. temperatureby heating
  2. customwas kept at 75° to 80° C
  3. additionAfter the addition
  4. custom(approximately 30 min.)
  5. temperaturethe reaction mixture was cooled to room temperature
  6. filtrationThe product was collected by filtration
  7. washthoroughly washed with water
  8. customto give

出典と根拠

ORDレコード
ord-80eb63ed89bd417c963e55eb57eaa4a7
出典データセット
uspto-grants-1984_06
特許番号
US04454362

関連ノート

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