Dichloroacetyl chloride → 1-Dichloroacetyl-4-n-propyl-piperazine

HRID 905139

反応式

HRID 905139 の反応式
C(=O)([O-])[O-].[K+].[K+].Br.Br.[CH2:9]([N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1)[CH2:10][CH3:11].[Cl:18][CH:19]([Cl:23])[C:20](Cl)=[O:21]>C(#N)C>[Cl:18][CH:19]([Cl:23])[C:20]([N:15]1[CH2:16][CH2:17][N:12]([CH2:9][CH2:10][CH3:11])[CH2:13][CH2:14]1)=[O:21]

参加物

5

反応物 3

HCID 6593Dichloroacetyl chlorideHCID 11430Potassium CarbonateHCID 3085288N-Propylpiperazinium dibromide

生成物 1

HCID 130141791-Dichloroacetyl-4-n-propyl-piperazine収率 96.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

21 g (0.15 mol) of potassium carbonate were added in portions to a suspension of 14.5 g (0.05 mol) of 1-n-propyl-piperazine dihydrobromide in 200 ml of acetonitrile. 7.4 g (0.05 mol) of dichloroacetyl chloride were added dropwise to this mixture at room temperature, while stirring. The mixture was subsequently stirred at 20° C. for 5 hours and working up was then effected by a procedure in which the reaction mixture was filtered and the filtrate was evaporated under reduced pressure. The residue was recrystallized from a mixture of toluene and petroleum ether. 11.5 g (96% of theory) of 1-dichloroacetyl-4-n-propyl-piperazine were obtained in the form of beige-colored crystals of melting point 88° C.

後処理

  1. stirringThe mixture was subsequently stirred at 20° C. for 5 hours
  2. filtrationwas filtered
  3. customthe filtrate was evaporated under reduced pressure
  4. customThe residue was recrystallized from a mixture of toluene and petroleum ether

出典と根拠

ORDレコード
ord-dfa14f1e76e84e3c8d17f332077698fe
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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