1-Acetylpiperazine → (4-Acetyl-piperazin-1-yl)pyridin-3-yl-acetic acid ethyl ester

HRID 352225

반응식

HRID 352225 반응식
[C:1]([N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1)(=[O:3])[CH3:2].[CH2:10]([O:12][C:13](=[O:22])[CH:14](Br)[C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[CH3:11]>>[CH2:10]([O:12][C:13](=[O:22])[CH:14]([N:7]1[CH2:8][CH2:9][N:4]([C:1](=[O:3])[CH3:2])[CH2:5][CH2:6]1)[C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[CH3:11]

참가 물질

3

반응물 2

HCID 837951-AcetylpiperazineHCID 21985933Ethyl 2-bromo-2-(pyridin-3-yl)acetate

생성물 1

HCID 69849407(4-Acetyl-piperazin-1-yl)pyridin-3-yl-acetic acid ethyl ester수율 60%

실험 절차

N-acetyl-piperazine (3.7 g; 28.8 mmol; 2.8 equiv) was combined with bromo-pyridin-3-yl-acetic acid ethyl ester (approx. 2.5 g; 10 mmol). Purification on a 3×16 cm silica column using a 30% then 40% ethyl acetate/hexanes (v/v) mobile phase followed by a 2% methanol/dichloromethane (v/v) mobile phase resulted in 1.84 g light yellow oil (approx. 60% yield). MS(ES) calc'd: [M+H]+=292.2 m/z; [M+Na]+=314.2 m/z.

후처리

  1. customPurification on a 3×16 cm silica column

출처 및 근거

ORD 기록
ord-5f7765389b5b496bb3641e9d3af6995f
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743794B2

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