Hydrochloric Acid → Pentachlorothiophenol

HRID 1462967

反応式

HRID 1462967 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 8620Pentachlorothiophenol

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
85 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-da1d455dfb354f818f19e32c4c1d6b7b
出典データセット
uspto-grants-1984_07
特許番号
US04461918

関連ノート

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