Sodium Bicarbonate → HCID 22464070, compound

Participants

Reaction Conditions

Reaction Steps

A stirred solution of the product from Step 1 (8.81 g, 0.0431 mol), under nitrogen, is treated with magnesium turnings (3.3 g) and kept for about 10 min when the solution became cloudy and an exothermic reaction began. It is stirred for an additional 5 min (23-24° C.), cooled to 6-7° C. in a water bath and kept for 5.5 h. This mixture is kept at 8° C. for 18 h, acidified to pH 3 with ice cold 6N HCl, neutralized with saturated NaHCO3, and extracted with EtOAc. The extracts are washed with water, dried (Na2SO4) and concentrated in vacuo to give 7.39 g of the titled product: MS (ES) m/z 193 (M+H+), 215 (17+Na+); 1H NMR (300 MHz, CDCl3); δ3.28 (m, 2H), 3.52 (broad s, 3H), 374 (s, 3H), 4.33 (q, 1H), 6.46 (m, 1H), 6.56 (m, 2H).

Provenance & Evidence