反应详情

In a flask were mixed together the above prepared 6-(1-isopropyl-piperidin-4-yloxy)-benzo[b]thiophene-2-carboxylic acid (0.147 g, 0.320 mmol, corrected for purity), 4,4-difluoropiperidine hydrochloride (0.060 g, 1.2 eq.), (benzotriazol-1-yloxy)-tris-(dimethylamino)phosphonium hexafluorophosphate (0.170 g, 1.2 eq.) and 2.5 eq. of N-ethyldiisopropylamine (0.760 mL) in 2 mL of abs. THF and allowed to react during one night at ambient temperature. Pouring onto crashed ice/AcOEt/NH4Cl-solution, twofold extraction with AcOEt, washing with water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, CH2Cl2/MeOH=9/1) produced 0.103 g of the title compound as white foam.

1. additionIn a flask were mixed together the
2. customto react during one night at ambient temperature
3. additionPouring
4. extractionextraction with AcOEt
5. washwashing with water and brine
6. dry with materialdrying over magnesium sulfate, and evaporation of the solvents