Triethylamine → Cyclopentanecarbonyl 4-(methyl)phenyl piperazine

HRID 417995ノート

反応式

HRID 417995 の反応式
Cl.Cl.[CH3:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.CCN(CC)CC.[CH:23]1([C:28](Cl)=[O:29])[CH2:27][CH2:26][CH2:25][CH2:24]1>C(Cl)Cl>[CH:23]1([C:28]([CH:11]2[CH2:12][NH:13][CH2:14][CH2:15][N:10]2[C:7]2[CH:6]=[CH:5][C:4]([CH3:3])=[CH:9][CH:8]=2)=[O:29])[CH2:27][CH2:26][CH2:25][CH2:24]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 78284Cyclopentanecarbonyl chlorideHCID 831121-(p-Tolyl)piperazine dihydrochloride

生成物 1

HCID 66650881Cyclopentanecarbonyl 4-(methyl)phenyl piperazine収率 98.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-Methylphenyl piperazine dihydrochloride (4.20 g, 16.9 mmol) and NEt3 (7.0 mL, 50.2 mmol) were dissolved in DCM (125 mL) at 0° C. Cyclopentanecarbonyl chloride (2.0 mL, 16.5 mmol) was added and the reaction mixture was allowed to warm to room temperature over 16 hours. The reaction mixture was washed with 1M aq Na2CO3 solution (3×100 mL), dried (MgSO4) and concentrated in vacuo to give cyclopentanecarbonyl 4-(methyl)phenyl piperazine (4.42 g, 98%) as a pale brown oil which was used without further purification.

後処理

  1. washThe reaction mixture was washed with 1M aq Na2CO3 solution (3×100 mL)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3297df9f01b645ad96f977418a0a8f14
出典データセット
uspto-grants-2012_01
特許番号
US08093248B2

反応ノート

読み込み中…