反应详情

0.46 ml of triethylamine and then 0.5 g of BOP are added to a mixture of 0.5 g of the compound obtained in EXAMPLE 11, step B), 0.127 g of phenylacetic acid and 10 ml of DCM. The resulting mixture is concentrated under vacuum and the residue is taken up with AcOEt, washed with water, with 1N NaOH solution and with saturated NaCl solution, dried over MgSO4 and concentrated under vacuum. The residue is chromatographed on silica gel H using DCM and then a DCM/MeOH mixture (94/6; v/v) as the eluent. The product obtained is taken up with DCM, acidified to pH 1 by the addition of hydrochloric ether and concentrated under vacuum to give 0.42 g of the expected hydrochloride after crystallization from iso ether. M.p.=125° C.

1. concentrationThe resulting mixture is concentrated under vacuum
2. washwashed with water, with 1N NaOH solution and with saturated NaCl solution
3. dry with materialdried over MgSO4
4. concentrationconcentrated under vacuum
5. customThe residue is chromatographed on silica gel H
6. customThe product obtained
7. concentrationconcentrated under vacuum