Benzene → Ethyl 1,4-dibenzylpiperazine-2-carboxylate

HRID 496036노트

반응식

HRID 496036 반응식
[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][NH:10][CH2:9][CH2:8][NH:7]1)=[O:5])[CH3:2].[CH2:12](N(CC)CC)C.CO[C:21]1[CH:32]=[CH:31][CH:30]=[CH:29][C:22]=1[C:23](Br)(OC)OC.[CH:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1>>[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][N:10]([CH2:23][C:22]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:21]=2)[CH2:9][CH2:8][N:7]1[CH2:12][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=[O:5])[CH3:2]

참가 물질

5

반응물 4

HCID 241Benzene2회HCID 8471TriethylamineHCID 10633257Ethyl Piperazine-2-carboxylateHCID 22324253Trimethoxy benzylbromide

생성물 1

HCID 2736402Ethyl 1,4-dibenzylpiperazine-2-carboxylate수율 44%

실험 절차

Piperazine 2-carboxylic acid ethyl ester (2.25 g, 14.25 mmol) was dissolved in dry benzene (30 ml) followed by addition of triehylamine (2.2 ml, 15.67 mmol). Trimethoxybenzyl bromide (3.72 g, 14.25 mmol) in dry benzene (30 ml) was added dropwise. The resulting mixture was stirred under nitrogen at room temperature overnight. The resulting salt was removed through filtration and solvent was evaporated. The crude product was purified by column chromatography using CH2Cl2:MeOH (15:1) to give the desired product in 44% yield.

후처리

  1. customThe resulting salt was removed through filtration and solvent
  2. customwas evaporated
  3. customThe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-6ea125ead655430eb0acd8e294cd7f58
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06943168B2

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