Hydrochloric Acid → 4-Chloro-2-nitrobenzoyl chloride

HRID 261898

反応式

HRID 261898 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](O)=[O:7])=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.S(Cl)([Cl:16])=O.Cl>CN(C)C=O>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([Cl:16])=[O:7])=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 804754-Chloro-2-nitrobenzoic acid

生成物 1

HCID 108677844-Chloro-2-nitrobenzoyl chloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
26 °C

実験手順

A mixture containing 1200 g. (5.95 moles) of 4-chloro-2-nitrobenzoic acid, 5000 ml. (69 moles) of thionyl chloride and 40 ml. of N,N-dimethylformamide was stirred 4 hours while the temperature was maintained at 26° C. When the evolution of hydrogen chloride subsided, the temperature was raised to 65° C. and stirring was continued an additional hour. After removing excess thionyl chloride by vacuum distillation, the residue was dissolved in 1 l. of 1,2-dichloroethane and the solution was evaporated under reduced pressure. The residue which was essentially free of thionyl chloride was dissolved in 5 l. of 1,2-dichloroethane and the solution was twice treated with decolorizing carbon and filtered to give a final solution of 4-chloro-2-nitrobenzoyl chloride in 1,2-dichloroethane which was used directly in the next step.

後処理

  1. additionA mixture containing 1200 g
  2. temperaturethe temperature was raised to 65° C.
  3. waitwas continued an additional hour
  4. customAfter removing excess thionyl chloride
  5. distillationby vacuum distillation
  6. dissolutionthe residue was dissolved in 1 l
  7. customof 1,2-dichloroethane and the solution was evaporated under reduced pressure
  8. dissolutionwas dissolved in 5 l
  9. additionof 1,2-dichloroethane and the solution was twice treated with decolorizing carbon
  10. filtrationfiltered

出典と根拠

ORDレコード
ord-2aba96c8fc6a472c913cc619c03e56de
出典データセット
uspto-grants-1979_05
特許番号
US04152518

関連ノート

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