反应详情

温度

80 °C

To a solution of (5R)-5-(5-(3-chloro-6,7-dihydro-5H-cyclopenta[b]pyridin-7-ylamino)-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepan-3-one (intermediate A22A) (62 mg, 146 μmmol) in dioxane (2.2 ml) at 23° C. was added 2,4-bis-(4-methoxy-phenyl)-[1,3,2,4]dithiadiphosphetane 2,4-disulfide (Lawesson's reagent) (38.3 mg, 94.6 μmmol) and the mixture was stirred at 80° C. for 3 h. The reaction mixture was poured onto sat. NaHCO3-solution and extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated to give a yellow solid, which was purified by silica gel column chromatography with n-heptane/ethyl acetate to give the (R)-5-[5-(3-chloro-6,7-dihydro-5H-[1]pyrindin-7-ylamino)-2-fluoro-phenyl]-6,6-difluoro-5-methyl-[1,4]oxazepane-3-thione (54 mg, 84%) as a white solid. MS (ISP): m/z=443.0 [(M+H)+].

1. extractionextracted twice with ethyl acetate
2. washThe combined organic layers were washed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. customevaporated
6. customto give a yellow solid, which
7. customwas purified by silica gel column chromatography with n-heptane/ethyl acetate