Hydrochloric Acid → HCID 86601368, compound

Participants

Reaction Conditions

Reaction Steps

1.24 g of the compound obtained in Stage C (4.21 mmoles) and 8.7 cm3 of ethyl acetate are placed in a 50 cm3 three-necked flask equipped with a magnetic stirrer and a temperature detector. The solution is cooled down to 0° C. then 8.7 cm3 of a saturated solution of gaseous HCl in ethyl acetate is added dropwise. Agitation is maintained for 5 minutes at 0° C. then the temperature of the solution is taken to 20° C. After agitating for two hours at 20° C., the solvent is evaporated off under reduced pressure in order to obtain a white powder to which an ethyl acetate/water mixture is added and a 20% solution of ammonium hydroxide is added. After dissolution and agitation for 10 minutes, decanting is carried out, followed by extracting again with 3× ethyl acetate. The organic phase is dried over MgSO4, filtered and rinsed with ethyl acetate. Finally, the solvent is evaporated off under reduced pressure in order to obtain 0.740 g of 4,5,6,7-tetrahydro-4-[(2-propenyloxy)amino]-isoxazolo[5,4-c]pyridine, of molecular formula C9H13N3O2 is obtained (M=195.22 g).

Provenance & Evidence