Chlorotrifluoroethylene → 3(2-Chloro-1,1,2-trifluoroethylthio) nitrobenzene

HRID 46623

反応式

HRID 46623 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([SH:10])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[OH-].[K+].[Cl:13][C:14]([F:18])=[C:15]([F:17])[F:16].ClC1C(C(F)(F)CF)=CC=CC=1[N+]([O-])=S>[Hg].CC(C)=O>[Cl:13][CH:14]([F:18])[C:15]([F:17])([F:16])[S:10][C:6]1[CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:9]=[CH:8][CH:7]=1

参加物

7

反応物 4

HCID 6594ChlorotrifluoroethyleneHCID 14797Potassium HydroxideHCID 2435763-Nitrobenzene-1-thiolHCID 178526931HCID 178526931、化合物

生成物 1

HCID 540174113(2-Chloro-1,1,2-trifluoroethylthio) nitrobenzene

試薬・触媒・溶媒 2

HCID 23931Mercury触媒HCID 180Acetone溶媒

実験手順

A mixture of 50 g. (0.322 moles) of 3-nitrothiophenol, 46.6 g. (0.402 moles) of potassium hydroxide, 60 ml. of acetone and 59 g. (0.395 moles) of 2-chloro-1,1,2-trifluoroethylene is heated in an autoclave with stirring for 11/2 hours at 60°-70° C. The reaction mixture is cooled, decanted and the solution evaporated to dryness in vacuo. The oily residue is combined with the solids, water is added and the product extracted with methylene chloride. The extracts are washed with 2.5 N aqueous sodium hydroxide and water, dried and evaporated to dryness in vacuo affording 76.5 g. of 3(2-chloro 1,1,2-trifluoroethylthio nitrobenzene with a b.p. at 0.25 mm. of mercury of 98°-102° C. The structure is verified with nuclear magnetic resonance.

後処理

  1. additionA mixture of 50 g
  2. temperatureThe reaction mixture is cooled
  3. customdecanted
  4. customthe solution evaporated to dryness in vacuo
  5. additionis added
  6. extractionthe product extracted with methylene chloride
  7. washThe extracts are washed with 2.5 N aqueous sodium hydroxide and water
  8. customdried
  9. customevaporated to dryness in vacuo
  10. customaffording 76.5 g

出典と根拠

ORDレコード
ord-52d400b817b54f0b9a95b00dd6f2ed59
出典データセット
uspto-grants-1979_11
特許番号
US04174400

関連ノート

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