反应详情

73.5 mg (0.60 mmol) of potassium carbonate are added to a mixture, prepared under argon, of 74.5 mg (0.35 mmol) of (3R)-quinuclidine-3-carbonyl chloride hydrochloride (Example 5A) and 60 mg (0.18 mmol) of 4′-amino-N-benzylbiphenyl-4-sulfonamide (Example 10A) in 2.2 ml of a 10:1 mixture of dioxane and DMF. After 18 h at 100° C., a further 74.5 mg. (0.35 mmol) of (3R)-quinuclidine-3-carbonyl chloride hydrochloride are added. After a further 24 h at 100° C., the reaction mixture is concentrated in vacuo. The residue is dissolved in water and acetonitrile and purified by preparative HPLC. The product fractions are concentrated, mixed with 5 ml of a 2:1 mixture of acetonitrile and 1 N hydrochloric acid, again concentrated and dried under high vacuum. 64 mg (70.5% of theory) of the title compound are obtained. HPLC (Method 1): Rt=4.17 min. MS (ESIpos): m/z=476 (M+H)+.

1. waitAfter a further 24 h at 100° C.
2. concentrationthe reaction mixture is concentrated in vacuo
3. dissolutionThe residue is dissolved in water
4. customacetonitrile and purified by preparative HPLC
5. concentrationThe product fractions are concentrated
6. additionmixed with 5 ml of a 2:1 mixture of acetonitrile and 1 N hydrochloric acid
7. concentrationagain concentrated
8. customdried under high vacuum