Formaldehyde → HCID 86760251, compound

Participants

Reaction Steps

3-[(3,4-Dichloro-benzyl-methyl-carbamoyl]-2-hydroxy-acrylic acid methyl ester (Compound 12-B) was treated with paraformaldehyde and methylamine thiophene as described in the preparation of Compound 12. The resulting residue was purified by chromatography (YMC Combiprep ODS-A, 30 mm×50 mm, MeOH/H2O/0.1% TFA) to yield the title compound as a white powder (58.7 mg, 28% yield). 1H NMR (300 MHz, CDCl3) δ: 7.41 (d, 1H, J=8.05), 7.33 (d, 1H, J=1.83), 7.26 (m, 1H), 7.08 (dd, 1H, J=8.05, J=1.83), 6.97 (m, 2H), 4.85 (s, 2H), 4.57 (s, 2H), 4.11 (s, 2H), 3.00 (s, 3H). HRMS (M−H) calcd for C18H15SN2Cl2O3: 409.0180. found: 409.0190.

Provenance & Evidence