Sodium Hydroxide → HCID 15767488, compound

Participants

Reaction Conditions

Reaction Steps

39.8 g (0.25 mol) 3-Amino-5-difluoromethoxy-1-methyl-pyrazole was dissolved in 224 ml water and 450 ml concentrated hydrochloric acid. At -10° C., 18.55 g (0.27 mol) sodium nitrite in 80 ml water was added dropwise. After stirring for 1 hour at -10° C., 137.6 g tin(II)chloride, dissolved in 180 ml concentrated hydrochloric acid, was added, dropwise, at this temperature. After a further hour stirring at -10° C., 805 ml 32% caustic soda was added dropwise at this temperature. The reaction mixture was shaken 8 times with ethyl acetate, the combined organic phases washed with saturated aqueous sodium chloride, dried over magnesium sulfate and concentrated.

Provenance & Evidence