反应 #88133
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04148895
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A stirred mixture of 8 g (0.02 mol) of 1-phenyl-2-(1-piperazinyl)-indole 3-carboxylic acid (4-methyl)-piperazide, 9.45 g (0.07 mol) of 2-(2-chloroethyl)-1,3-dioxolane and 9.7 ml of triethylamine in 60 ml of toluene was maintained at the boil for 40 hours. After cooling, the mixture was diluted with 200 ml of chloroform, washed three times with water, and the solvent was eliminated in vacuo. The resinous residue of the organic phase was chromatographed using silica gel 60 (0.06-0.2 mm, deactivated by 10% of water, column size: 3 × 100 cm) with chloroform containing 10% methanol. The base was eluted as a resin. The yield amounted to 6.6 g (66% of the theoretical yield). The dihydrochloride melted at 215°-217° C. was maintained at the boil for 40 hours After cooling washed three times with water The resinous residue of the organic phase was chromatographed The base was eluted as a resin theoretical yield)
来源 ID: ord-2ea726274d5b438283d3b7d1fe3bc327