反应详情

温度

0 °C

To a round bottom flask equipped with a magnetic stir bar was added 4-chloro-7H-pyrrolo[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (0.13 g, 0.58 mmol, 1.0 eq.) and DMF (3 ml). The mixture was cooled to 0° C. followed by the addition of NaH (0.028 g, 0.70 mmol, 1.2 eq) with stirring. After stirring for 10 minutes SEM-CL (0.106 g, 0.64 mmol, 1.1 eq) was added and the reaction was allowed to warm to room temperature with stirring for 1 hour. The reaction was diluted with ethyl acetate (50 ml), washed (2×) water, (1×) NaHCO3, (2×) 5% LiCl, (1×) brine, and dried over sodium sulfate, and concentrated in vacuo to give 4-chloro-7-(2-trimethylsilanyl-ethoxymethyl)-7H-pyrrolo[2,3-d]pyrimidine-6-carboxylic acid ethyl ester as a cream solid (0.17 g, 84%). MS (ESI) for C15H22ClN3O3Si: 356 (MH+).

1. customTo a round bottom flask equipped with a magnetic stir bar
2. additionwas added
3. temperatureto warm to room temperature
4. stirringwith stirring for 1 hour
5. washwashed (2×) water, (1×) NaHCO3, (2×) 5% LiCl, (1×) brine
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated in vacuo