Dichloroacetyl chloride → ST50911991

HRID 905138

反応式

HRID 905138 の反応式
[Cl:1][CH:2]([Cl:6])[C:3](Cl)=[O:4].[N+:7]([C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)=[CH:12][CH:11]=1)([O-:9])=[O:8].C(N(CC)CC)C>C1(C)C=CC=CC=1>[N+:7]([C:10]1[CH:11]=[CH:12][C:13]([N:16]2[CH2:21][CH2:20][N:19]([C:3](=[O:4])[CH:2]([Cl:6])[Cl:1])[CH2:18][CH2:17]2)=[CH:14][CH:15]=1)([O-:9])=[O:8]

参加物

5

反応物 3

HCID 6593Dichloroacetyl chlorideHCID 8471TriethylamineHCID 804471-(4-Nitrophenyl)piperazine

生成物 1

HCID 2837846ST50911991収率 46%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

7.1 g (0.048 mol) of dichloroacetyl chloride were added dropwise to a solution of 10 g (0.048 mol) of 1-(4-nitrophenyl)-piperazine and 5 g (0.495 mol) of triethylamine in 100 ml of toluene at room temperature, while stirring. The mixture was subsequently stirred at 20° C. for 3 hours. Working up was then effected by a procedure in which the reaction mixture was washed twice with 100 ml of water each time and the organic phase was separated off, dried and evaporated under reduced pressure. The residue was recrystallized from toluene. 7 g (46% of theory) of 1-(4-nitrophenyl)-4-dichloroacetyl-piperazine were obtained in the form of light yellow crystals of melting point 155° C.

後処理

  1. stirringThe mixture was subsequently stirred at 20° C. for 3 hours
  2. washwas washed twice with 100 ml of water each time
  3. customthe organic phase was separated off
  4. customdried
  5. customevaporated under reduced pressure
  6. customThe residue was recrystallized from toluene

出典と根拠

ORDレコード
ord-a2ca27a80e8c43d2b6bf33d8d91bd5aa
出典データセット
uspto-grants-1983_12
特許番号
US04422866

関連ノート

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