Hydrochloric Acid → 2-(3-bromo-1H-pyrazol-1-yl)ethan-1-ol

Potassium tert-butoxide in THF (0.510 mL, 0.510 mmol) was added to a solution of 3-bromo-1H-pyrazole (50.0 mg, 0.340 mmol) in DMF (3 mL) and stirred at r.t. for 10 min, and then 1,3,2-dioxathiolane 2,2-dioxide (0.0633 g, 0.510 mmol) was added and the stirred at r.t. for 1 h. At this time, conc. HCl (0.3 mL) was added to the above reaction mixture and then stirred at r.t. overnight. The mixture was diluted with ethyl acetate, washed with saturated NaHCO3, water and brine, dried over Na2SO4, filtered, and concentrated to give the crude product which was directly used in the next reaction without further purification. LCMS (M+H)+: m/z=191.0.

1. stirringthe stirred at r.t. for 1 h
2. stirringstirred at r.t. overnight
3. washwashed with saturated NaHCO3, water and brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated

ORDレコード

ord-ddab1f1833374d4f9d20640487b75a10

出典データセット

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08436008B2