Sodium Carbonate → HCID 18509406, compound

Participants

Reaction Steps

Compound 142 (0.28 g; 7.66×10−1 mmol) and phosphorus oxychloride (0.59 g; 3.83 mmol) was added dropwise to pyridine (15 ml), and the mixture was refluxed for 2 hours. The mixture was brought to room temperature, and poured into ice/water. The pH of the mixture was adjusted to weak alkaline by use of sodium carbonate, followed by extraction with chloroform (50 ml). The organic layer was washed with saturated aqueous sodium bicarbonate solution and then with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1), to thereby yield 0.18 g of the target compound (yield: 67.6%).

Provenance & Evidence