反应详情

温度

0 °C

Ethyl 4-ethyl-1-[5-[2-(3-ethyl-5-methyl-2-oxo-1,3,5-triazinan-1-yl)-7-(3-hydroxyprop-1-ynyl)-1,3-benzothiazol-5-yl]pyrimidin-2-yl]piperidine-4-carboxylate (325 mg, 0.55 mmol) was dissolved in anhydrous DCM (32 mL) under argon and the solution cooled to 0° C. Triethylamine (0.19 mL, 1.40 mmol) was added followed by methanesulfonyl chloride (0.064 mL, 0.82 mmol) and the mixture allowed to warm to rt and stirred for 45 minutes. The mixture was diluted with water, extracted into DCM (3×20 mL) and the combined organic layer washed with brine, dried over Na2SO4 and concentrated to dryness under reduced pressure. The desired compound was obtained as a yellow oil which was used without further purification in the next step. MS: 670.09 [M+H]+.

1. temperatureto warm to rt
2. extractionextracted into DCM (3×20 mL)
3. washthe combined organic layer washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to dryness under reduced pressure