反应详情

温度

100 °C

Degas a stirred mixture of 6-(4-bromo-3-fluorobenzylthio)-3-tert-butoxycarbonyl-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine (212 mg, 0.424 mmol), 5-fluoro-2-methoxybenzene boronic acid (108 mg, 0.636 mmol), potassium carbonate (292 mg, 2.12 mmol), triphenylphosphine (11 mg, 0.0424 mmol) and bis(triphenylphosphine)-palladium(II) chloride (15 mg, 0.0212 mmol) in dioxane (3 mL) and water (1 mL). Purge with dry nitrogen and heat at 100° C. for 5 h. Cool to ambient temperature, add water, extract three times with EtOAc, dry over anhydrous Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1) to give 3-tert-butoxycarbonyl-7-chloro-6-(2,5′-difluoro-2′-methoxy-biphenyl-4-ylmethylthio)-2,3,4,5-tetrahydro-1H-benzo[d]azepine as yellow oil (216 mg, 93%). Use a method similar to the General Procedure 1-4 to give the title compound as a yellow foam. MS (ES+) m/z: 446 (M+H)+.

1. customDegas
2. customPurge with dry nitrogen
3. temperatureCool to ambient temperature
4. additionadd water
5. extractionextract three times with EtOAc
6. dry with materialdry over anhydrous Na2SO4
7. concentrationconcentrate in vacuo
8. customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1)