反应 #2071639
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04800203
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a suspension of phthalimidopyrrole (748.6 g) and 2,4-dichlorobenzoyl chloride (1109.1 g) in 3.5 L of dichloroethane was added 707.3 g of K-10 Montmorillonite clay. The resulting mixture was stirred at reflux for 48 hrs, then filtered and concentrated to a semisolid. The semisolid was triturated with a large quantity of ether and collected to yield 112.5 g of powder. The ether wash was concentrated to give 162.0 of a residue. This was purified by high performance liquid chromatography (HPLC hereinafter, silica, dichloromethane) and recrystallized from absolute ethanol to yield 37.26 g of crystals, mp 152°-153° C. at reflux for 48 hrs filtered concentrated to a semisolid The semisolid was triturated with a large quantity of ether collected
来源 ID: ord-756f8d01a25a4f3aa590e7b5ab821c91