Sodium Hydroxide → HCID 16124640, compound

Participants

Reaction Conditions

Reaction Steps

Compound 3 (2.8 g, 10.2 mmol) was dissolved in ortho-phosphoric acid (40 ml). The mixture was heated to 150° C. for 18 hours, and the intended product confirmed by LC-MS. The mixture was cooled to 0° C. and the acid neutralized with concentrated NaOH. Extraction with methylene chloride afforded a mixture of Compounds 4 and 4′, which was then purified by HPLC to provide Compound 4 (180 mg, 9%). 1H NMR (400 MHz, CD3OD) δ 9.16 (d, J=7.8 Hz 1 H) 8.48 (s, 1 H) 7.62 (d, J=7.8 Hz 1 H) 7.52 (d, J=6.8 Hz 1 H) 7.44 (m, 2 H). [M+H] calc'd for C17H12N2, 245; found 245.

Provenance & Evidence