Water → HCID 68461384, compound

Participants

Reaction Steps

The product from Example 185d was dissolved in 50% HCl:H2O and heated to 100° C. for 1 hr. Reaction mixture was then cooled to room temperature, made basic with 2N NaOH, and extracted with CH2Cl2. Dried over Na2SO4, filtered and concentrated under vacuum giving the crude title compound. Purified by HPLC with TFA providing the product as a trifluoroacetic acid (87 mg, 64%). 1H NMR (300 MHz, DMSO-d6) δ ppm: 0.98 (t, J=7.35 Hz, 3 H), 1.79-1.92 (m, J=7.43, 7.43, 7.43, 7.43, 7.43 Hz, 2 H), 2.32 (s, 3 H), 3.00 (t, J=7.54 Hz, 2 H), 6.34 (d, J=6.99 Hz, 1 H), 6.49 (t, J=7.54 Hz, 1 H), 6.68 (d, J=6.99 Hz, 1 H), 6.92 (d, J=8.09 Hz, 1 H), 7.05-7.13 (m, 1 H), 7.15-7.20 (m, 1 H), 7.24 (d, J=8.46 Hz, 1 H), 7.28 (s, 1 H), 7.84 (d, J=8.82 Hz, 1 H), 8.42 (d, J=6.99 Hz, 1 H), 9.06 (d, J=8.82 Hz, 1 H); MS (ESI+) m/z 401 (M+H−TFA)+; (ESI−) m/z 399 (M−H−TFA)−.

Provenance & Evidence