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Hydrochloric Acid → N,N-Diethyl-4-phenylpiperazine-1-carboxamide--hydrogen chloride (1/1)

HRID 543475
ノート
印刷プレビュー

反応式

HRID 543475 の反応式
[C:1]1([N:7]2[CH2:12][CH2:11][N:10]([C:13](=[O:19])[N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:20]>C(Cl)(Cl)Cl>[ClH:20].[C:1]1([N:7]2[CH2:8][CH2:9][N:10]([C:13](=[O:19])[N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH2:11][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 423348HCID 423348、化合物

生成物 1

HCID 20461509N,N-Diethyl-4-phenylpiperazine-1-carboxamide--hydrogen chloride (1/1)収率 70.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

In 50 ml of chloroform was dissolved 2.6 g (0.01 mole) of 1-phenyl-4-diethylcarbamoylpiperazine at room temperature, and the solution was saturated with gaseous hydrogen chloride and stirred for a certain time. The solvent was removed by distillation under reduced pressure. Then, 50 ml of acetone was added to the residue and the mixture was stirred for a certain time. The precipitated crystal was recovered by filtration, washed with acetone, stirred in 50 ml of acetone to effect washing and dried to obtain 2.1 g of 1-phenyl-4-diethylcarbamoylpiperazine hydrochloride having a melting point of 190° to 192° C. The yield was 70.9%. The elementary analysis values are as follows.

後処理

  1. customThe solvent was removed by distillation under reduced pressure
  2. additionThen, 50 ml of acetone was added to the residue
  3. stirringthe mixture was stirred for a certain time
  4. filtrationThe precipitated crystal was recovered by filtration
  5. washwashed with acetone
  6. stirringstirred in 50 ml of acetone
  7. washto effect washing
  8. customdried

出典と根拠

ORDレコード
ord-9d2b228f5648472cbe6fa64313a46713
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04446133

反応ノート

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