Sodium methanethiolate → HCID 10476716, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of compound 6 (24.4 mg, 0.061 mmol) and sodium thiomethoxide (8 mg, 0.1 mmol) in DMF (1.5 mL) was heated for 22 h at 110° C. After cooling, the reaction mixture was concentrated to dryness and the residue was purified by a silica gel column chromatography (chloroform-methanol, 20:1) to give compound 16 (13 mg, 52.0%) as a colorless solid. 1H NMR (DMSO-d6) δ 3.06 (s, 6 H, N(CH3)2), 3.56 (s, 3 H, CH3), 4.58 (br s, 2 H, CH2), 7.10 (pseudo t, J=7.9 and 7.6 Hz, 1 H, H-16), 7.38 (d, J=7.6 Hz, 1 H, H-17), 7.56 (d, J=7.9 Hz, 1 H, H-15), 7.76 (s, 1 H, H-13), 7.69 (s, 1 H, H-8), 7.90 (br s, 1 H, exchangeable with D2O, NH).

Provenance & Evidence