Potassium Phosphate, Tribasic → HCID 66696717, compound

Participants

Reaction Steps

A mixture of Example 36A (870 mg, 3.40 mmol), Pd(OAc)2 (38.1 mg, 0.170 mmol), tricyclohexylphosphine (95 mg, 0.34 mmol), K3PO4 (2524 mg, 11.9 mmol), and cyclopropylboronic acid (379 mg, 4.42 mmol) in toluene (16 mL) and water (0.8 mL) was heated in a microwave reactor at 100° C. for 1.5 hr. A second, identical reaction was performed. The two reactions were combined, and then filtered, rinsed with EtOAc, and concentrated to an orange oil. The crude product was chromatographed on silica gel (Analogix® SF25-40G column, 0%-25% EtOAc/hexanes, 30 mL/min), which yielded 1.37 g (93%) of the title compound as yellow crystals. 1H NMR (300 MHz, CH3OH-d4) δ 8.13 (s, 1H), 7.35 (dd, J=8.1, 1.8 1H), 7.29 (dd, J=11.4, 1.8 1H), 7.06 (t, J=8.0, 1H), 2.39 (s, 3H), 2.17-2.05 (m, 1H), 1.03 (dd, J=8.5, 6.4, 4.3 2H), 0.81-0.73 (m, 2H). MS (DCI+) m/z 218 (M+H).

Provenance & Evidence