3209-71-0, Isoxazole-3-carboxylic Acid is a Isoxazoles compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
[00226] Isooxazole-3 -carboxylic acid ((8′), 92 wt % assay based on 1H-NMR, 3.86 kg, 34.1 mol, 1.0 equiv), toluene (19.3 L) and DMF (0.131 L, 1.69 mol, 0.05 equiv) were mixed in a 30 L jacketed reaction vessel equipped with a nitrogen inlet-outlet, overhead stirrer, a thermocouple and an addition funnel. The resulting slurry was heated to 45 to 55 C. Oxalyl chloride (4.80 kg, 37.8 mol, 1.11 equiv) was charged via the addition funnel over the course of 4 hours 30 minutes, while maintaining the reaction temperature between 45 to 55 C. Vigorous gas evolution was observed. A brown mixture was obtained after the addition. The brown mixture was held at 45 to 55 C for 30 minutes, then heated to 85 to 95 C and stirred at 85 to 95 C for 1 hour. During heating, the brown mixture turned into a black mixture. The black mixture was cooled to 20 to 25 C, over 4 hours and held at 20 to 25 C for a minimum of 16 hours. The reaction was monitored by quenching a portion of the reaction mixture into piperidine and monitoring the formation of the piperidine amide by HPLC ((8′) : piperidine amide area:area % was < 1.9). After the reaction was complete by HPLC the dark mixture was in-line filtered via gas a dispersion tube (coarse frit) into a 20 L rotavapor flask. Toluene (3.9 L) was used to rinse the reactor and the rinse was in-line filtered into the 20 L rotavapor flask. The filtered reaction mixture was concentrated under reduced pressure until no more distillate was seen coming off.
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Reference£º
Patent; CYCLERION THERAPEUTICS, INC.; WALLACE, Debra Jane; ZHOU, Fenger; WANG, Yuguang; NAKAI, Takashi; KARNATI, Vishnu Vardhan Reddy; SCHAIRER, Wayne C.; KISSEL, Willaim; XUE, Song; HASHASH, Ahmad; (263 pag.)WO2019/140095; (2019); A1;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem