反応 #170690

ord-d4b6b70399b9472ebdbce97fd404ebe8

反応方程式

C=C(CCC(=O)OC)C(=O)OC
2-methylenepentanedioic acid dimethyl ester
COc1ccc(CN)c(OC)c1
2,4-dimethoxybenzylamine
COC(=O)C1CCC(=O)N(Cc2ccc(OC)cc2OC)C1
titled compound
COC(=O)C1CCC(=O)N(Cc2ccc(OC)cc2OC)C1
1-(2,4-Dimethoxybenzyl)-6-oxopiperidine-3-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
  2. 2
    洗浄washed with a 1M aqueous solution of hydrochloric acid, water
  3. 3
    乾燥a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate
  4. 4
    濃縮concentrated under reduced pressure

実験手順

To a solution of 2-methylenepentanedioic acid dimethyl ester (19.2 g) in toluene (195 ml) was added 2,4-dimethoxybenzylamine (16.6 ml), and the mixture was stirred for 3 days at reflux. This reaction solution was cooled to room temperature, and then washed with a 1M aqueous solution of hydrochloric acid, water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give a crude product of the titled compound (26.8 g).

出典

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