Methylamine → HCID 10453217, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of compound 6 (25 mg, 0.06 mmol) and 2M methylamine in THF (1 mL) and 40% methylamine in water (1 mL) was stirred for 14 h at 85° C. After removal of volatiles in vacuo, the residue was triturated with methanol-water, and the solid that formed was collected by suction filtration, washed with water (10 mL), and dried to give compound 11 (22 mg, 89.0%). 1H NMR (DMSO-d6) δ 2.76 (d, J=4.6 Hz, 3 H, NHCH3), 3.55 (s, 3 H, 9-CH3), 4.59 (br s, 2 H, CH2), 6.28 (br d, J=4.3 Hz, 1 H, exchangeable with D2O, NHCH3), 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), 7.57 (d, J=7.6 Hz, 1 H, H-15), 7.67 (s, 1 H, H-13), 7.35 (s, 1 H, H-8), 7.83 (br s, 1 H, exchangeable with D2O, NH).

Provenance & Evidence