Formaldehyde → HCID 68115436, compound

Participants

Reaction Conditions

Reaction Steps

A 25-mL round-bottom flask containing 19.1 (19 mg, 0.04 mmol, 1.00 equiv), formic acid (1 mL) and formaldehyde (37%, 5 mL) was heated at 100° C. for 12 h in an oil bath under nitrogen. The mixture was concentrated under reduced pressure and the residue (45 mg) purified by preparative HPLC(SHIMADZU) under the following conditions: column: Xbridge Prep C18, 19*150 mm 5 um; mobile phase: water (0.05% NH4HCO3) and CH3CN (5.0% CH3CN up to 53.0% in 16 min); UV detection at 254 and 220 nm. The product-containing fractions were collected and evaporated under reduced pressure to afford compound I-31 (5.7 mg, 37%) as an off-white oil. 1H NMR (300 MHz, CDCl3) δ 1.20 (m, 3H), 1.54 (m, 4H), 1.61 (m, 1H), 2.02-2.80 (m, 14H), 2.28-3.10 (m, 2H), 3.48 (m, 5H), 5.24 (m, 1H), 8.50 (s, 1H). MS: m/z 390 (M+H)+.

Provenance & Evidence