反应 #3698271
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05003081
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 19.8 g of malononitrile were dissolved in 30 ml of DMF and cooled to 0° C. While cooling, 61 g of triethylamine and 27 g of chloroacetyl chloride were simultaneously added dropwise to this, and the mixture was stirred at 10° C. for 10 minutes. 65.7 g of tridecylamine were then added dropwise, and the reaction mixture was stirred at room temperature for 48 hours. 300 ml of isopropylamine were then added to the mixture, which was refluxed for 2 hours, 10 g of active carbon were added, and the mixture was filtered hot. After cooling, the precipitate was filtered off with suction, washed and dried at 50° C. 40 g (44% of theory) of the compound of the formula ##STR25## of melting point 214° to 215° C. were obtained. The IR, NMR, UV and mass spectra and the elemental analysis are consistent with the structural formula. While cooling the reaction mixture was stirred at room temperature for 48 hours was refluxed for 2 hours 10 g of active carbon were added the mixture was filtered hot After cooling the precipitate was filtered off with suction washed dried at 50° C 40 g (44% of theory) of the compound of the formula ##STR25## of melting point 214° to 215° C. were obtained
来源 ID: ord-4d2a89e19e394fb7bae643ae04a07e93