反应 #2151081
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05366969
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5 g 3,4-Dihydropyrido-(1,2-a)-pyrimidin-2-one (Fluka) were melted at 80° C. with 5.5 g H3PO4 and mixed, while stirring, with 5.9 ml PCl3. After 20 hours at the given temperature, it was mixed with 70 ml 2N HCl, stirred for 8 hours at 100° C. and, after cooling, filtered off from the undissolved part. The filtrate was evaporated on a rotary evaporator and purified by ion exchanger chromatography on Amberlite IR 120 (H+ form) with water as eluent. The fractions obtained after electrophoresis were evaporated in a vacuum and the oil remaining behind, after dissolving in a little water, brought to crystallisation by the addition of acetone. mixed after cooling filtered off from the undissolved part The filtrate was evaporated on a rotary evaporator purified by ion exchanger chromatography on Amberlite IR 120 (H+ form) with water as eluent The fractions obtained after electrophoresis were evaporated in a vacuum after dissolving in a little water brought to crystallisation by the addition of acetone
来源 ID: ord-d0c17a9469564c4e942518a3886b630a