反応 #170765

ord-c90155ae579c439c8ebb8b7b6b0a8244

反応方程式

C=C(C(=O)OC)C1(C(=O)OC)CC1
1-(1-methoxycarbonylvinyl)cyclopropanecarboxylic acid methyl ester
COc1ccc(CN)c(OC)c1
2,4-dimethoxybenzylamine
COC(=O)C1CN(Cc2ccc(OC)cc2OC)C(=O)C12CC2
titled compound
COC(=O)C1CN(Cc2ccc(OC)cc2OC)C(=O)C12CC2
5-(2,4-Dimethoxybenzyl)-4-oxo-5-azaspiro[2.4]heptane-7-carboxylic acid methyl ester

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度at reflux for 20 hours
  2. 2
    濃縮This reaction mixture was concentrated under reduced pressure
  3. 3
    その他the resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1)

実験手順

To a solution of 1-(1-methoxycarbonylvinyl)cyclopropanecarboxylic acid methyl ester (720 mg) in toluene (3.6 ml) was added 2,4-dimethoxybenzylamine (587 μl) at room temperature, and then the mixture was stirred at reflux for 20 hours. This reaction mixture was concentrated under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1) to give the titled compound (567 mg).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846746B2uspto-grants-2014_09