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ChemicalBook CAS DataBase List 7-METHYLBENZO[D]ISOXAZOL-3-OL
36238-83-2

7-METHYLBENZO[D]ISOXAZOL-3-OL synthesis

3synthesis methods
-

Yield:36238-83-2 93%

Reaction Conditions:

with di-isopropyl azodicarboxylate;triphenylphosphine in tetrahydrofuran at 20; for 0.533333 h;Inert atmosphere;Mitsunobu Displacement;

Steps:

Typical procedure

General procedure: Salicylhydroxamic acid 1a (77 mg, 0.5 mmol, 1 equiv) was dissolved in anhydrous THF (7 mL) under an inert (N2) atmosphere. Triphenylphosphine (164 mg, 0.625 mmol, 1.25 equiv) was then added. After 2 min, DIAD (123 lL, 0.625 mmol, 1.25 equiv) was added dropwise. TLC (Hex/EtOAc, 1:3) after 30 min revealed the reaction was complete. The THF was removed in vacuo. The residue was partitioned between 0.1 M NaOH (50 mL)and CH2Cl2 (100 mL). The organic layer was separated, then the aqueous layerwas washed a further three times with CH2Cl2 (100 mL). The aqueous layer was acidified with 1 M HCl (10 mL), then extracted into CH2Cl2 (2 100 mL),washed with brine (50 mL), dried (Na2SO4), filtered and concentrated to yield the 3-hydroxybenzisoxazole 2a.

References:

Van Eker, Daniel;Chauhan, Jay;Murphy, William A.;Conlon, Ivie L.;Fletcher, Steven [Tetrahedron Letters,2016,vol. 57,# 48,p. 5301 - 5303]

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