Purification of Laboratory Chemicals, Fifth Edition

"ORGANIC CHEMICALS: H" HARMINE

[442-51-3] M 212.3, m 261 (dec), pK 20 7.61. Crystd from MeOH.

Harmine hydrochloride (hydrate) [343-27-1] M 248.7, m 280 (dec). Crystd from water.

Hecogenine acetate [915-35-5] M 472.7, m 265-268 , [ ?] 23 D -4.5 (c 1, CHCl 3). Crystd from MeOH.

Heptadecanoic acid (margaric) [506-12-7] M 270.5, m 60-61 , b 227 /100mm, pK Est 4.9. Crystd from MeOH or pet ether.

1-Heptadecanol [1454-85-9] M 256.5, m 54 . Crystd from acetone.

Heptafluoro-2-iodopropane [677-69-0] M 295.9, b 41 . Purified by gas chromatography on a triacetin (glyceryl triacetate) column, followed by bulb-to-bulb distn at low temperature. Stored over Cu powder to stabilise it.

n-Heptaldehyde [111-71-7] M 114.2, b 40.5 /12mm, 152.8 /760mm, d 0.819, n 25 1.4130. Dried with CaSO 4 or Na 2SO 4 and fractionally distd under reduced pressure. More extensive purification by pptn as the bisulfite compound (formed by adding the aldehyde to saturated aqueous NaHSO 3) which was filtered off and recrystd from hot H 2O. The crystals, after being filtered and washed well with H 2O, were hydrolysed by adding 700mL of aqueous Na 2CO 3 (12.5% w/w of anhydrous Na 2CO 3) per 100g of aldehyde. The aldehyde was then steam distd, separated, dried with CuSO 4 and distd under reduced pressure in a slow stream of nitrogen. [McNesby and Davis J Am Chem Soc 76 2148 1954].

n

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