Sulfuric Acid → HCID 67314636, Verbindung

A solution of 5-fluoro-1,3-dihydro-indol-2-one (141 mg, 0.93 mmol.) in THF (4 mL) is treated with a solution of lithium bis(trimethylsilyl)amide (1.9 mL of a 1 M solution in THF, 1.9 mmol) dropwise. The resulting solution is stirred at room temperature for 10 min. A solution of 2-(2,2-dimethoxy-ethyl)-7H-furo[3,4-b]pyridin-5-one (104 mg, 0.47 mmol in THF (1 mL) is added dropwise to the reaction mixture. The resulting solution is stirred for 1.5 h and is then poured into cold aqueous 2N H2SO4 solution (10 mL) at 0° C. The resulting mixture is heated at 45° C. for 30 min and then cooled to room temperature and stirred overnight. The reaction mixture is poured into ice water (150 mL) and stirred for 2h. The solid which formed is collected to give the title compound as a brown solid (76 mg, 46%).

1. stirringThe resulting solution is stirred for 1.5 h
2. temperatureThe resulting mixture is heated at 45° C. for 30 min
3. temperaturecooled to room temperature
4. stirringstirred overnight
5. stirringstirred for 2h
6. customThe solid which formed
7. customis collected

ORD-Eintrag

ord-0798566e85ab462c8bd865c4a799c977

Quelldatensatz

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07977351B2