6-Chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione → HCID 12297296, compound

Participants

Reaction Steps

A solution of sodium hydrosulphide hydrate (74.77 g, 1335.243 mmol) in water (125 ml) was added dropwise to a stirred solution of Step 1 (50.0 g, 286.532 mmol) in chloroform (250 ml) and ethanol (636 ml) in an ice water bath, and the mixture was stirred at room temperature overnight. The reaction mixture was evaporated to dryness in vacuo at room temperature. The residue obtained was dissolved in water (100 ml) and extracted with dichloromethane (2×100 ml). The aqueous layer was acidified with 1 N HCl. Precipitated solid was filtered, washed with water (2×100 ml) and dried to obtain 49.22 g of the product as a pale yellow solid; 1H NMR (300 MHz, CDCl3) δ 3.33 (s, 3H), 3.74 (s, 3H), 4.17 (s, 2H).

Provenance & Evidence