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

HRID 496036ノート

反応式

HRID 496036 の反応式
[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]

参加物

5

反応物 4

HCID 241Benzene2 回HCID 8471TriethylamineHCID 10633257Ethyl Piperazine-2-carboxylateHCID 22324253Trimethoxy benzylbromide

生成物 1

HCID 2736402Ethyl 1,4-dibenzylpiperazine-2-carboxylate収率 44%

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-6ea125ead655430eb0acd8e294cd7f58
出典データセット
uspto-grants-2005_09
特許番号
US06943168B2

反応ノート

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