反应详情

温度

60 °C

A mixture of 2-aza-bicyclo[3.1.0]hexane hydrochloride (example 4 step 7, 49 mg, 1.2 eq.) and potassium carbonate (118 mg, 2.5 eq.) in acetonitrile was stirred 1 h at 60° C. The reaction mixture was cooled to 30° C. and [5-(3-chloro-propoxy)-1H-indol-2-yl]-morpholin-4-yl-methanone (example 4, step 3, 110 mg, 1.0 eq.) was added. The resulting mixture was stirred 24 h at 80° C. The reaction mixture was partitioned between ethyl acetate and water. The aqueous layer was extracted with ethyl acetate and the combined organic layers were washed with an aqueous solution of sodium hydrogencarbonate and water and dried over sodium sulphate and evaporated in vacuo. The residue was purified on silica, eluting with a 98:2 to 9:1 gradient of dichloromethane/methanol, to yield 12 mg (8%) of the desired product as light yellow solid. MS (m/e): 370.4 (MH+, 100%).

1. temperatureThe reaction mixture was cooled to 30° C.
2. stirringThe resulting mixture was stirred 24 h at 80° C
3. customThe reaction mixture was partitioned between ethyl acetate and water
4. extractionThe aqueous layer was extracted with ethyl acetate
5. washthe combined organic layers were washed with an aqueous solution of sodium hydrogencarbonate and water
6. dry with materialdried over sodium sulphate
7. customevaporated in vacuo
8. customThe residue was purified on silica
9. washeluting with a 98:2 to 9:1 gradient of dichloromethane/methanol