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

HRID 10778

반응식

HRID 10778 반응식
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]

참가 물질

5

반응물 3

HCID 6367Acetyl chloride2회HCID 11430Potassium Carbonate2회HCID 804471-(4-Nitrophenyl)piperazine

생성물 1

HCID 28651491-Acetyl-4-(4-nitrophenyl)piperazine수율 722.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-994cbfeb630d41b6b2862208213baf98
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094896B2

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