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With lithium hydroxide monohydrate; water; at 25℃; for 6.5h;Large scale;
An aqueous solution of lithium hydroxide monohydrate (124.5 kg of a solution preparedfrom 49.44 kg lithium hydroxide monohydrate dissolved in 319 kg water, 398 mol) was added to asolution of <strong>[118994-89-1]ethyl 5-oxazolecarboxylate</strong> (54 kg, 382.7 mol) in water (54 kg) maintaining the temperature below 25 C. The reaction was stirred for 6.5 h and then conc. aqueous HCI (64.8 kg) was added maintaining the temperature below 25 C, the crystallisation cooled to 5 C and held forh. The product was filtered off, washed with cold water (88 kg), then isopropanol (171 kg) anddried under vacuum at 50 C to give the title compound (37.88 kg, 87.S%).1H NMR (400 MHz, DMSO-d6) ppm 13.68 (br. 5., 1 H), 8.59 (5, 1 H), and 7.88 (5, 1 H).
87.5%
With lithium hydroxide monohydrate; In water; at 25℃; for 6.5h;Large scale;
An aqueous solution of lithium hydroxide monohydrate (124.5 kg of a solution prepared from 49.44 kg lithium hydroxide monohydrate dissolved in 319 kg water, 398 mol) was added to a solution of <strong>[118994-89-1]ethyl 5-oxazolecarboxylate</strong> (54 kg, 382.7 mol) in water (54 kg) maintaining the temperature below 25 C. The reaction was stirred for 6.5 h and then cone, aqueous HCI (64.8 kg) was added maintaining the temperature below 25 C, the crystallisation cooled to 5 C and held for 1 h. The product was filtered off, washed with cold water (88 kg), then isopropanol (171 kg) and dried under vacuum at 50 C to give the title compound (37.88 kg, 87.5%). (0437) *H NMR (400 MHz, DMSO-cfe) delta ppm 13.68 (br. s., 1 H), 8.59 (s, 1 H), and 7.88 (s, 1 H).
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