3-IODO-1-METHYL-1H-PYRAZOLE

The compound N-methyl-3-aminopyrazole (2000 g, 20.6 mol, 1.0 eq) was dissolved in 6000 ml of concentrated hydrochloric acidAnd 2000 ml of water, Cooled to 0-5 ° C in an ice-salt bath, Then, 3.5 L of a saturated aqueous sodium nitrite solution (NaNO2, 2842.8 g, 41.2 mol, 2.0 eq) was added dropwise, After mechanical stirring reaction for 20 min, The reaction solution was added dropwise to an aqueous solution of 8000 ml of potassium iodide (8549.0 g, 51.5 mol, 2.5 eq) at 0 ° C, After completion of the dropwise addition, The reaction was allowed to spontaneously rise to room temperature for 4 h, After TLC detection reaction was complete, Add ethyl acetate extraction 2 times, The organic phase was dried with saturated brine and concentrated, The crude product was purified via flash column to give compound 3-iodo-l-methyl-lH-pyrazole (3473.8 g, 16.7 mol)Yield 81.0percent.To a suspension of l-methyH/f-pyrazol-3-amine (200 mg, 2.06 mmol) in THF (5 mL) under The compound N-methyl-3-aminopyrazole (2000 g, 20.6 mol, 1.0 eq) was dissolved in 6000 ml of concentrated hydrochloric acidAnd 2000 ml of water, Cooled to 0-5 ° C in an ice-salt bath, Then, 3.5 L of a saturated aqueous sodium nitrite solution (NaNO2, 2842.8 g, 41.2 mol, 2.0 eq) was added dropwise, After mechanical stirring reaction for 20 min, The reaction solution was added dropwise to an aqueous solution of 8000 ml of potassium iodide (8549.0 g, 51.5 mol, 2.5 eq) at 0 ° C, After completion of the dropwise addition, The reaction was allowed to spontaneously rise to room temperature for 4 h, After TLC detection reaction was complete, Add ethyl acetate extraction 2 times, The organic phase was dried with saturated brine and concentrated, The crude product was purified via flash column to give compound 3-iodo-l-methyl-lH-pyrazole (3473.8 g, 16.7 mol)Yield 81.0percent.To a suspension of l-methyH/f-pyrazol-3-amine (200 mg, 2.06 mmol) in THF (5 mL) under

Molecular Weight:208.00
XLogP3:0.9
Hydrogen Bond Acceptor Count:1
Exact Mass:207.94975
Monoisotopic Mass:207.94975
Topological Polar Surface Area:17.8
Heavy Atom Count:7
Complexity:66.7
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes