Die Isolierung des Urothions

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Abstract
1000 1. urine were stirred for 10 min. with 2 kg. "Carborafnn C" (charcoal). After standing 1 hr., the sediment was separated, treated with 2.5 1. 50% NaOH and filtered. After washing with 10 1. H2O, it was eluted with 15 1. acetone-NH3 (1 part acetone, 4 parts H2O, 1 part 2N NH3). The eluate was concd. to 2 1. in vacuo, neutralized with 2 N H2SO4, and filtered through a Buchner funnel containing 400 g. fuller''s earth XXF. The filter cake was washed with 2 1. H2O and then with 50% acetone. The acetone filtrate was collected and the portion containing the pigment (about 1 1.) concd. in vacuo to 300 cc. The soln. was adjusted to about pH 7.6 with phosphate buffer, filtered through 350 g. of the fuller''s earth, and the pigment eluted with 11. 0.15 M borate buffer, pH 9.2. The eluate was concd. to about 500 cc, 20 cc. 10% HgSO4 in 2 N H2SO4 added, the precipitate formed suspended in 250 cc. N/10 H2SO4 and decomposed with H2S. The mixture was filtered, the filtrate made alkaline with Na2CO3 and concd. in vacuo to 100 cc. The alkaline soln. was warmed to 60[degree], filtered and weakly acidified with acetic acid at 60[degree]-80[degree], and the urothion obtained as reddish-yellow clusters of needles or less well formed crystals. The recrystallized urothion (CuHisOsNuSa) was almost insoluble in organic solvents, but somewhat soluble in H2O, aqueous alkalis and strong acids. In 0.05 N NaOH, the optical rotation of urothion was, ([alpha])D=[long dash]12[degree].

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