Hydrochloric Acid → 3,5-Dichloro-4-methylaniline

HRID 1462647

反応式

HRID 1462647 の反応式
Cl[C:2]1[C:8]([Cl:9])=[C:7]([CH3:10])[C:6]([Cl:11])=[C:5](Cl)[C:3]=1[NH2:4].C1(O)C=CC=CC=1.[H][H].Cl>[Pd].O.C1(C)C=CC=CC=1.[Ta]>[Cl:9][C:8]1[CH:2]=[C:3]([CH:5]=[C:6]([Cl:11])[C:7]=1[CH3:10])[NH2:4]

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 996PhenolHCID 202734132,3,5,6-Tetrachloro-4-methylanilineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 6411543,5-Dichloro-4-methylaniline収率 98%

試薬・触媒・溶媒 4

HCID 23938Palladium触媒HCID 23956Tantalum触媒HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

61.5 parts of 2,3,5,6-tetrachloro-4-methylaniline, 180 parts of phenol and 15 parts of a 1% strength palladium/charcoal catalyst are reacted with hydrogen under a maximum pressure of 50 bar at 180° C. in a tantalum autoclave, in the presence of a small amount of hydrochloric acid, in the course of 5 hours, while stirring. After the pressurized vessel has been cooled and the pressure released, the mixture is diluted with 300 parts of water and 200 parts of toluene, rendered alkaline, heated to 90°, and separated from the catalyst. The catalyst is boiled up with toluene, and the combined toluene solutions are distilled. 44 parts of 3,5-dichloro-4-methylaniline, bp. 146°-155°/18 mbar, 98% strength, are obtained; yield: 98% of theory.

後処理

  1. temperatureAfter the pressurized vessel has been cooled
  2. temperatureheated to 90°
  3. customseparated from the catalyst
  4. distillationthe combined toluene solutions are distilled

出典と根拠

ORDレコード
ord-a41c7d8b657f4d07aacb21eb4aa4fd25
出典データセット
uspto-grants-1984_07
特許番号
US04460788

関連ノート

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