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Purification of Laboratory Chemicals, 8th Edition by W.L.F. Armarego

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2-Chloro-3,5-dinitropyridine [2578-45-2] C5H2ClN3O3, M 203.5, m 62-65°, 63-65°, 64°, pKEst <-5. Dissolve it in CHCl3, shake it with saturated NaHCO3, dry (MgSO4), evaporate and apply to an Al2O3 column, elute with petroleum ether (b 60-80°), evaporate and recrystallise it from *C6H6 or petroleum ether. [Ochiai & Kaneko Chem Pharm Bull Jpn 8 28 1960, DOI: org/10.1248/cpb.8.28; Plazek Recl Trav Chim Pays-Bas 72 569 1953, DOI: 10.1002/recl.19530720706; Beilstein 20/5 V 458.]

1-(2-Chloroethyl)pyrrolidine hydrochloride [7250-67-1] C6H12Cl.HCl, M 170.1, m 167-170°, 173.5-174°, pKEst ~ 8.5 (free base). Purify the hydrochloride by recrystallisation from isopropanol/di-isopropyl ether (charcoal) and recrystallise it twice more. The free base, b 55-56°/11mm, ...

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