1-Bromo-2-Chloroethane → 4-Bromo-1-(2-chloroethyl)-1H-pyrazole

Temperature

60 °C

4-Bromopyrazole (700 mg, 4.76 mmol, available from Aldrich), cesium carbonate (2328 mg, 7.14 mmol, available from Aldrich) and 1-bromo-2-chloroethane (0.592 ml, 7.14 mmol, available from Acros) were suspended in N,N-dimethylformamide (DMF) (14 ml) and heated to 60° C. under microwave conditions in an Emrys Optimiser for 1 hour. The mixture was partitioned between water (20 ml) and ethyl acetate (60 ml). The aqueous layer was run off and the organic washed (water ×3 (10 ml), brine (10 ml)), dried (magnesium sulfate) and evaporated to dryness to give the desired compound (868 mg).

1. customThe mixture was partitioned between water (20 ml) and ethyl acetate (60 ml)
2. washthe organic washed (water ×3 (10 ml), brine (10 ml))
3. dry with materialdried (magnesium sulfate)
4. customevaporated to dryness

ORD record

ord-796f6094ed244866b8fc3624646b4d12

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08697725B2