Hydrochloric Acid → Pentachlorothiophenol

HRID 1462967

반응식

HRID 1462967 반응식
[Cl:1][C:2]1[C:7](Cl)=[C:6]([Cl:9])[C:5]([Cl:10])=[C:4]([Cl:11])[C:3]=1[Cl:12].[SH-:13].[Na+].[OH-].[Na+].Cl>O.CN(C)C=O>[Cl:1][C:2]1[C:7]([SH:13])=[C:6]([Cl:9])[C:5]([Cl:10])=[C:4]([Cl:11])[C:3]=1[Cl:12]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8370HexachlorobenzeneHCID 14798Sodium HydroxideHCID 28015Sodium hydrosulfide

생성물 1

HCID 8620Pentachlorothiophenol

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
85 °C

실험 절차

Hexachlorobenzene (25.0 g, 0.088 mol) was added to 50 mL of dimethylformamide followed by the addition of 7.4 g (0.096 mol) of 73% sodium hydrosulfide and 7.9 mL (0.079 mol) of 40% aqueous sodium hydroxide. The stirred reaction mixture was heated to 85° C. for 3.0 hr, cooled to room temperature, and poured into 200 mL of water. After 10 min of stirring, the insoluble material was removed by filtration, and the filtrate acidified with 15 mL (0.18 mol) of concentrated aqueous hydrochloric acid. The resulting precipitate was collected by filtration, washed with 100 mL of water, and dried in vacuo giving 22.8 g, 92% of theoretical, of pentachlorothiophenol.

후처리

  1. customThe stirred reaction mixture
  2. temperaturecooled to room temperature
  3. customthe insoluble material was removed by filtration
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with 100 mL of water
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-da1d455dfb354f818f19e32c4c1d6b7b
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04461918

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