1-Methylpiperazine → HCID 131715415, compound

Participants

Reaction Conditions

Reaction Steps

2-Carboxymethyl-1-(4'-fluorophenyl)-5-trifluoromethylindolin-3-on (15 g) and MgCl2. 6H2O (30 g) in HMPA (100 ml) were heated under N2 at 120°-140° C. for 1 h and finally at 150° C. for another 1/2 h. 1-Methylpiperazin (25 ml) was added and the mixture was refluxed under N2 at an oil bath temperature of 200° C. for 16 h. The mixture was cooled and poured into 1 ltr. of H2O and extracted with ether (3×200 ml). The combined ether extracts were washed with 0.5 M HCl (3×300 ml). The acidic H2O phase was made alkaline and reextracted with ether (2×200 ml). The combined organic phase was dried (MgSO4) and the ether evaporated. The remaining oil was dissolved in acetone and the title compound precipitated as a dihydrochloride. Yield: 6.7 g (35%). M.p. 245°- 247° C.

Provenance & Evidence