反应详情

Sodium azide (492 mg, 7.5688 mmol) was added portion wise to a stirred solution of 7-fluoro-6-(trifluoromethyl)-2,3-dihydro-1H-inden-1-one (I-77c: 500 mg, 2.2935 mmol) in TFA (15 mL) over a period of 5 hours at 80° C. The reaction was monitored by TLC (5% methanol in CHCl3). The reaction mixture was concentrated under reduced pressure, followed by the addition of ice. The precipitated solid was filtered, washed with water (20 mL) and dried under reduced pressure to yield the crude product. Purification by column chromatography on silica gel (2% methanol in CHCl3) afforded 300 mg of the product (56.1% yield).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionfollowed by the addition of ice
3. filtrationThe precipitated solid was filtered
4. washwashed with water (20 mL)
5. customdried under reduced pressure
6. customto yield the crude product
7. customPurification by column chromatography on silica gel (2% methanol in CHCl3)