反应详情

温度

25 °C

A suspension of 5-chloro-pyrazine-2-carboxylic acid (prepared as in Example 29, 1.00 g, 6.33 mmol) in methylene chloride (30 mL) was treated with 1,3-dibenzyloxy-2-propanol (2.06 g, 7.57 mmol), bis(2-oxo-3-oxazolidinyl)phosphinic chloride (1.61 g, 6.34 mmol), and triethylamine (1.83 mL, 12.66 mmol). The mixture was stirred at 25° C. overnight. The solution was extracted with methylene chloride and a saturated aqueous sodium bicarbonate solution. The organic layer was washed with water, a saturated aqueous sodium chloride solution, a 1N aqueous hydrochloric acid solution, and a saturated aqueous sodium chloride solution. The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. Biotage chromatography (FLASH 40L, Silica, 3/1 hexanes/ethyl acetate) afforded the 5-chloropyrazine-2-carboxylic acid 2-benzyloxy-1-benzyloxymethyl-ethyl ester (1.45 g, 55.7%) as a colorless oil.

1. extractionThe solution was extracted with methylene chloride
2. washThe organic layer was washed with water
3. dry with materialThe organic layer was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo