反应详情

To a solution of ethyl 4-(4-methyl-piperazin-1-ylmethyl)-3-trifluoromethyl-benzoate (7.23 g, 21.1 mmol, 1.0 eq.) in ethanol (40 ml) is added 1M NaOH (30.6 ml, 30.6 mmol, 1.4 eq.). After stirring for 2 h at room temperature a clear pale yellow solution is obtained. The mixture is evaporated to a volume of 30 ml. Then, the solution is adjusted to pH 7 by addition of 1M HCl and the solvent is stripped off. The residue is taken up three times in toluene (70 ml) and evaporated. The crude material is dissolved in ethanol/THF 1:9 (150 ml), filtered, evaporated, triturated with ethyl acetate, and vacuum dried at 60° C. over night to afford a beige powder: HPLC: tR=3.61 min (purity: >99%, gradient A), ESI-MS: 303.3 [MH]+

1. customis obtained
2. customThe mixture is evaporated to a volume of 30 ml
3. additionThen, the solution is adjusted to pH 7 by addition of 1M HCl
4. customevaporated
5. dissolutionThe crude material is dissolved in ethanol/THF 1:9 (150 ml)
6. filtrationfiltered
7. customevaporated
8. customtriturated with ethyl acetate, and vacuum
9. customdried at 60° C. over night
10. customto afford a beige powder