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温度

0 °C

To a suspension of phosphorus pentasulfide (27 g) in dry THF (100 ml) at 0° C. under vigorous stirring, Na2CO3 (13 g) was added. The reaction mixture was stirred for 30 min at 0° C. and for 30 min at r.t., then diethoxyacetamide (6 g) was added and stirring was continued at r.t. for 70 h. The reaction was then diluted with EA, washed with 10% Na3PO4, brine, dried over Na2SO4 and the solvent removed in vacuo. The crude residue was purified by flash-chromatography (EE/PE 1/1) to give the title compound as a white solid (4.4 g).

1. additionwas added
2. stirringstirring
3. waitwas continued at r.t. for 70 h
4. washwashed with 10% Na3PO4, brine
5. dry with materialdried over Na2SO4
6. customthe solvent removed in vacuo
7. customThe crude residue was purified by flash-chromatography (EE/PE 1/1)