Acetyl chloride → 1-Acetyl-4-(4-nitrophenyl)piperazine

HRID 10778

反応式

HRID 10778 の反応式
C(=O)([O-])[O-].[K+].[K+].[C:7](Cl)(=[O:9])[CH3:8].[N+:11]([C:14]1[CH:19]=[CH:18][C:17]([N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[CH:16][CH:15]=1)([O-:13])=[O:12]>ClCCl>[C:7]([N:23]1[CH2:24][CH2:25][N:20]([C:17]2[CH:16]=[CH:15][C:14]([N+:11]([O-:13])=[O:12])=[CH:19][CH:18]=2)[CH2:21][CH2:22]1)(=[O:9])[CH3:8]

参加物

5

反応物 3

HCID 6367Acetyl chloride2 回HCID 11430Potassium Carbonate2 回HCID 804471-(4-Nitrophenyl)piperazine

生成物 1

HCID 28651491-Acetyl-4-(4-nitrophenyl)piperazine収率 722.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Powdered potassium carbonate (276 mg, 2 mmol) and then acetyl chloride (0.14 mL, 2 mmol) were added to a solution of 1-(4-nitrophenyl) piperazine (2.1 g, 1 mmol) (Acros Organics) in dichloromethane (75 mL). The mixture was stirred at room temperature overnight and then further quantities of powdered potassium carbonate (500 mg, 3.6 mmol) and acetyl chloride (0.2 mL, 2.8 mmol) were added. The mixture was stirred at room temperature overnight, then it was filtered and the filter cake was washed with dichloromethane. The solvent was evaporated from the filtrate, and the residue was chromatographed (0–66% acetone/dichloromethane) to give 1-acetyl-4-(4-nitrophenyl)piperazine (1.8 g, 72%).

後処理

  1. stirringThe mixture was stirred at room temperature overnight
  2. filtrationit was filtered
  3. washthe filter cake was washed with dichloromethane
  4. customThe solvent was evaporated from the filtrate
  5. customthe residue was chromatographed (0–66% acetone/dichloromethane)

出典と根拠

ORDレコード
ord-994cbfeb630d41b6b2862208213baf98
出典データセット
uspto-grants-2006_08
特許番号
US07094896B2

関連ノート

読み込み中…