L-Tartaric acid → 2,3-Dihydroxybutanedioic Acid

Temperature

60 °C

[4-(5-aminomethyl-2-fluoro-phenyl)-piperidin-1-yl]-[7-fluoro-1-(2-methoxy-ethyl)-4-trifluoromethoxy-1H-indol-3-yl]-methanone (0.250 g, 0.554 mmol) was weighed in a 20 ml glass vial. A solution of L-(+)-tartaric acid at 2.66 mmol/ml in 5:1 (v/v) acetonitrile/water was prepared, and 0.2084 ml of this solution was added to the weighed solid with stirring and heating to ˜60° C. giving a clear solution. The solution was then evaporated in vacuo on a rotary evaporator leaving a glassy solid which was recrystallized in hot isopropyl acetate to which a minimum amount of isopropanol was added to give a clear solution. Upon cooling the crystalline product was isolated by filtration and dried in vacuo at room temperature.

1. customgiving a clear solution
2. customThe solution was then evaporated in vacuo on a rotary evaporator
3. customleaving a glassy solid which
4. customwas recrystallized in hot isopropyl acetate to which a minimum amount of isopropanol
5. additionwas added
6. customto give a clear solution
7. temperatureUpon cooling the crystalline product
8. customwas isolated by filtration
9. customdried in vacuo at room temperature

ORD record

ord-87d341b0d6b24360984172ee02f7e402

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08497379B2