反应详情

温度

80 °C

154 mg (0.46 mmol) N-[3-(2-ethoxy-2-hydroxyacetyl)-phenyl]-benzenesulphonamide (Component I) and 125 mg (0.48 mmol) methyl 1-(3-amino-3-methyl-butyl)-indole-5-carboxylate (Component IV) are dissolved in 10 ml of ethanol and combined with 4 drops of triethylamine. The reaction solution is heated to 80° C. for 17 hours. Then it is cooled to 0° C. and over a period of 2.5 hours 140 mg (3.7 mmol) sodium borohydride are added batchwise. The mixture is stirred for another hour at 0° C. and the reaction solution is then poured into a mixture of 20 ml of saturated aqueous potassium carbonate solution and 50 ml of ethyl acetate. After separation of the organic phase the aqueous phase is extracted with ethyl acetate. The combined organic phases are with washed saturated aqueous saline solution and dried on sodium sulphate. Then the solvent is eliminated in vacuo and the residue is chromatographed on silica gel (DCM/methanol=100:0:0→9:1).

1. additionare added batchwise
2. customAfter separation of the organic phase the aqueous phase
3. extractionis extracted with ethyl acetate
4. customdried on sodium sulphate
5. customthe residue is chromatographed on silica gel (DCM/methanol=100:0:0→9:1)