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Potassium Carbonate → 2-Chloro-3-[2-ethyl-4-(phenylmethyl)-1-piperazinyl]pyrazine

HRID 991671
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HRID 991671 반응식
Cl[C:2]1[C:7]([Cl:8])=[N:6][CH:5]=[CH:4][N:3]=1.[CH2:9]([N:16]1[CH2:21][CH2:20][NH:19][CH:18]([CH2:22][CH3:23])[CH2:17]1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH2:9]([N:16]1[CH2:21][CH2:20][N:19]([C:2]2[C:7]([Cl:8])=[N:6][CH:5]=[CH:4][N:3]=2)[CH:18]([CH2:22][CH3:23])[CH2:17]1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 785752,3-DichloropyrazineHCID 220365411-Benzyl-3-ethylpiperazine

생성물 1

HCID 220363902-Chloro-3-[2-ethyl-4-(phenylmethyl)-1-piperazinyl]pyrazine수율 71%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 2,3-dichloropyrazine (3.9 g, 27 mmol), 1-benzyl-3-ethylpiperazine (4.6 g, 22.5 mmol; from Step 1) and K2CO3 (6.2 g, 45 mmol) in DMF (10 mL) was stirred at 100° C. for 4 days. The solvent from the filtered reaction mixture was evaporated off and the residue was purified by column chromatography on silica using heptane/EtOAc (90:10) as eluent to yield 5.0 g (71%) of the title compound as a light yellow oil. HRMS m/z calcd for C17H21ClN4 (M)+ 316.1455, found 316.1448.

후처리

  1. customThe solvent from the filtered reaction mixture
  2. customwas evaporated off
  3. customthe residue was purified by column chromatography on silica

출처 및 근거

ORD 기록
ord-e489cca6207c4706a9cad9133db08e9b
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06465467B1

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