1,2-Dichloroethane → HCID 18783777, compound

Participants

Reaction Steps

EDC (636 mg, 3.3 mmol) was added to a solution of the compound of Example 8(b) (682 mg, 3.3 mmol), ethyl-4-carboxypiperidine acetate 14 (646 mg, 3 mmol), HOBt. H2O (446 mg, 3.3 mmol) and DIEA (1.2 mL, 6.8 mmol) in anhydrous DMF (10 mL) at RT. After stirring for 20 h, the reaction was concentrated on rotavap (high vacuum). The resulting residue was taken into EtOAc and washed successively with H2O (3×20 mL), 10% NaHCO3 (2×20 ml) and saturated NaCl. The organic extract was dried (anhydrous Na2SO4), filtered and concentrated to yield the title compound (350 m g, 32%) as a yellow solid. HPLC k' 5.3 (Ultrasphere® ODS, gradient , A:acetonitrile B:water-0. 1% trifluoroacetic acid, 5-60% acetonitrile during 20 min; UV detection at 220 nm). MS (ESI) m/e 368.2[M+H]+.

Provenance & Evidence