6-{(Acetyloxy)methyl}pyridin-3-yl acetate (36.59 g, 174.90 mmol) was dissolved in concentrated hydrochloric acid (36%, 400 ml). The black solution was stirred at reflux (110°C) for 24 h. After cooling to ambient temperature, the solvent was removed under reduced pressure until around 50 ml remained. An aqueous solution of sodium hydroxide (1 M) was added dropwise to neutralise the solution (pH 7.0). All solvent was then removed under reduced pressure and the crude brown-grey solid was dried overnight in vacuo at 50°C. The crude solid was then stirred in boiling acetonitrile (250 ml) and filtered hot. This process was repeated a further two times (2 × 250 ml). The yellow-pale brown filtrates were combined and the acetonitrile was removed under reduced pressure to leave the product as a yellow solid, which was dried overnight in vacuo. Yield = 15.81 g, 126.35 mmol, 72%.

¹H NMR (400 MHz, 298 K, DMSO) δ_H 9.72 (1H, br s, Py-OH), 8.02 (1H, d, ⁴J_HH = 3.0 Hz, Py), 7.26 (1H, d, ³J_HH = 8.5 Hz, Py), 7.15 (1H, dd, ³J_HH = 8.5 Hz, ⁴J_HH = 3.0 Hz, Py), 5.19 (1H, br s, CH₂OH), 4.44 (1H, s, CH₂).

¹³C{¹H} NMR (100 MHz, 298K, DMSO) δ_C 152.2 (Py), 152.0 (Py), 136.3 (Py), 122.5 (Py), 121.0 (Py), 63.9 (CH₂).

MS (ESI) m/z 126.1 [M+H]⁺, 148.1 [M+Na]⁺, 124.1 [M-H]^-.

IR v cm^-1 3439 w, 2407 w, 1765 w, 1570 m, 1483 m, 1461 m, 1445 m, 1335 m, 1270 s, 1209 s, 1127 m, 1117 m, 1072 s, 1027 m, 893 m, 858 m, 830 s, 760 m, 714 m, 656 s.

Elemental Analysis found (Calculated for C₆H₇NO₂) % C 57.73 (57.59), H 5.51 (5.64), N 10.87 (11.19).