Category: 3405-77-4

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3405-77-4,5-Methylisoxazole-3-carboxylic acid,as a common compound, the synthetic route is as follows.

5-Methylisoxazole-3-carboxylic acid (150 mg, 1.18 mmol) dissolved in toluene (2 mL) was treated with DMF (1 drop) and thionyl chloride (1.42 mmol, 103 Iota then heated to reflux for 5 h. The solvent was removed in vacuo to afford crude 5-methylisoxazole-3- carbonyl chloride (155 mg, 1.06 mmol) as a brown oil. The crude acid chloride without purification was dissolved in THF (4 mL), treated with Et3N (155 mu, i.o6 mmol) and stirred for 5 min, before adding 4-(2-aminoethyl)benzenesulfonamide (220 mg, 1.10 mmol) and stirring at room temperature for 15 h under N2 atmosphere. The reaction mixture was concentrated in vacuo and purified by MPLC, affording the titled compound as an amorphous white solid (205 mg, 62%): NMR (600 MHz, DMSO- d6) delta 8.79 (t, J = 5-8 Hz, lH), 7-74 (d, J = 8.3 Hz, 2H), 7.41 (d, J = 8.3 Hz, 2H), 7.30 (s, 2H), 6.50 (q, J= 0.8 Hz, lH), 3.49 (m, 2H), 2.91 (t, J = 7.2 Hz, 2H), 2.45 (d, J= 0.8 Hz, 3H); ^C NMR (151 MHz, DMSO-d6) delta 171.0, 158.8, 158.5, 143-3, 142.0, 129.0, 125. 6, 101.1, 39-8, 34-3, H-7; HRMS (ESI-TOF) m/z calcd for C13H14N304S [M-H]- 308.0711, found 308.0708; LC-MS m/z 308.0 [M+H]+, purity >99% (ELSD).

The synthetic route of 3405-77-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; THE UNIVERSITY OF QUEENSLAND; THE PROVOST, FELLOWS, FOUNDATION SCHOLARS, AND THE OTHER MEMBERS OF BOARD, OF THE COLLEGE OF THE HOLY AND UNDIVIDED TRINITY OF QUEEN ELIZABETH NEAR DUBLIN; O’NEILL, Luke; COLL, Rebecca; COOPER, Matthew; ROBERTSON, Avril; SCHRODER, Kate; MACLEOD, Angus Murray; MILLER, David John; (109 pag.)WO2018/215818; (2018); A1;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3405-77-4,5-Methylisoxazole-3-carboxylic acid,as a common compound, the synthetic route is as follows.

2-3 (6.9 g, 54.0 mmol) was dissolved in dry DCM (300 mL) at 0 C.Oxalyl chloride (7.0 mL, 81.0 mmol) was added dropwise. Subsequently, a catalytic equivalent of DMF is added,Stir for 20 minutes, warm to room temperature and stir for 2 h.After the reaction was completed, the solvent was concentrated under reduced pressure and the obtained acid chloride was applied to the next step without purification.Compound 2-2 was dissolved in dry DCM, and the pH of the TEA was adjusted to 7.0 at 0 C, and the acid chloride prepared above was added dropwise.After stirring for 10 minutes, TEA (23.0 mL, 162 mmol) was added dropwise.Raise to room temperature and stir for 2 h. When the reaction is complete, use water, saturated citric acid,The organic phase was washed with saturated NaHCO3 and saturated sodium chloride. The combined organic phases were dried over anhydrous sodium sulfate.The solvent was evaporated under reduced pressure, and the obtained crude product was purified by flash column (PE: EA = 5:1).Compound 2-4 was obtained as a yellow oil (14 g, yield 80%).

The synthetic route of 3405-77-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Nankai University; Shang Luqing; Ma Yuying; He Shuai; Shang Chengyou; (32 pag.)CN110105348; (2019); A;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem

3405-77-4, 5-Methylisoxazole-3-carboxylic acid is a Isoxazoles compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 87. Synthesis of S-fS-Methylisoxazole-theta-CarboxamidoV^-ChlorobenzoicAcid (Intermediate 42)42[0280] Ethyl S-methylisoxazole-S-carboxylate (500 mg, 3.22 mmol) was suspended in MeOH-THF-H2O (2OmL, 1:1:1) and lithium hydroxide monohydrate (1.35 g, 32.2 mmol) was added. The reaction mixture was stirred for 16 h at room temperature, and acidified with IN HCl. The crude product was extracted with ethyl acetate, and ethyl acetate layer was dried (Na2SO4) and solvent evaporated. The white solid thus obtained, was suspended in dichloromethane (30 mL) and treated with thionyl chloride (2.35 mL, 32.3 mmol) at reflux for 6 hr. The reaction mixture was evaporated, and the residue was dissolved in hexane-ethyl acetate mixture (100 mL, 6:4) and quickly filtered through a short silica plug. On evaporation of solvent, 5-methylisoxazole-3-carbonyl chloride was obtained as a colorless syrup (330 mg, 70%).[0281] qTo a solution of 5-amino-2-chlorobenzoic acid (342 mg, 2.0 mmol) and TEA (1.39 mL, 10 mmol), was added 5-methylisoxazole-3-carbony. chloride (300 mg, 2.06 mmol) in DCM (5 mL). The reaction mixture was stirred at room temperature for 16 hr, and triturated with aqueous sodium bicarbonate. The organic layer was separated, dried (Na2SO4) and evaporated. The residue on filtered through a silica plug to give the title compound as a cream colored solid (330 mg, 57%).

As the paragraph descriping shows that 3405-77-4 is playing an increasingly important role.

Reference£º
Patent; TARGEGEN, INC.; WO2008/8234; (2008); A1;,
Isoxazole – Wikipedia
Isoxazole | C3H3NO – PubChem