反应 #3017064
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09029189B2
反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a 100 mL flask, 0.4078 g of di-(2-aminopropyl)amine (0.00311 mol) was dissolved in 50 mL of 1-methylnaphthalene. Carbon disulfide (0.18 mL, 0.00298 mol) was added. The reaction was stirred for three hours then heated to 200° C. The reaction was heated for four days until production of hydrogen sulfide stopped. The solvent was then removed by distillation. The product was then dissolved in approximately 5 mL of hexanes and 0.5 mL of a 2.0 M ether solution of hydrogen chloride was added. The yield of the precipitate was 0.278 g (53%). The NMR had a doublet at 1.19 ppm, a multiplet at 3.44 ppm, a multiplet at 3.92 ppm and a multiplet at 4.15 ppm. The solvent was then removed by distillation The product was then dissolved in approximately 5 mL of hexanes 0.5 mL of a 2.0 M ether solution of hydrogen chloride was added
来源 ID: ord-0668a5a0741b4e9b93abf1899e8ce733