反应详情

温度

50 °C

A solution of (1H-imidazol-4-yl)methanol (14.6 g, 108 mmol) in DMF (100 mL) was treated with imidazole (22.16 g, 325 mmol) and TBDPSCl (29.8 g, 108 mmol) and the mixture was stirred and heated to 50° C. for 6 h. It was then allowed to cool to RT, poured onto H2O and extracted with DCM. The combined org. layers were dried over Na2SO4, filtered and concentrated in vacuo. Purification by flash chromatography (SiO2, DCM/MeOH 100:0 to 90:10) afforded the title compound (35.3 g). UPLC-MS: MS 337.2 (M+H+); UPLC rt 1.04 min.

1. temperatureto cool to RT
2. additionpoured onto H2O
3. extractionextracted with DCM
4. dry with materiallayers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification by flash chromatography (SiO2, DCM/MeOH 100:0 to 90:10)