59669-59-9, 3-(tert-Butyl)isoxazol-5-amine is a Isoxazoles compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,59669-59-9
Step 7: Synthesis of compound D-8Activation of 60 g (0.25 mol) of compound D-7as the corresponding acid chloride is achieved by treatment with thionyl chloride (0.9 L, 12.39 mol) at 60 ¡ãC for 1.5 h. The reaction is cooled to room temperature and acid chloride mixture was evaporated to dryness. The acid chloride mixture is dissolved in DCM (200 mL).This acid chloride solution is added dropwise over 20 mins to a stirred suspension of 36 g (0.25 mol) of 3-tert-butyl-isoxazol-5-ylamine and 0.6 L (0.50 mol) of N,N- diisopropylethylamine in DCM (400 mL) at 35 ¡ãC. After complete addition the reaction is stirred at room temprature for 17 h. The solvent is removed under reduced pressure. The residue is purified by dry-flash column chromatography (silica, eluent heptanes, 20percent ethyl acetate) to yield 50 g of light brown solid. Solid is re-crystallized from (50percent IPA in heptane) to afford 34 g of compound D-8 Yield: 43percent; ES-MS: m/z 359 [M+H];’H-NMR (400 MHz, CHLOROFORM-d) delta ppm 1.33 (9 H, s), 1.76 (6 H, s), 1.83 – 1.91 (2H, m), 1.92 – 2.05 (2 H, m), 3.34 – 3.51 (3 H, m), 4.07 (2 H, ddd, 7=11.86, 2.20, 2.08 Hz), 6.27 (1 H, s), 9.60 (1 H, s)
The synthetic route of 59669-59-9 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; HICKEY, Eugene Richard; RIETHER, Doris; ERMANN, Monika; WO2012/12307; (2012); A1;,
Isoxazole – Wikipedia
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