Hydrochloric Acid → 21243-09-4

2-Fluorothiophenol (5.0 g, 39 mmol) was dissolved in tetrahydrofuran (50 ml) under a nitrogen atmosphere. Triethylamine (3.94 g, 5.33 ml, 85.8 mmol) was added. Acrylic acid (2.81 g, 2.67 ml, 39 mmol) was dissolved in tetrahydrofuran and added dropwise to the reaction solution over 2 h at room temperature. The mixture was stirred at room temperature overnight. 1M Hydrochloric acid (50 ml) was added and the phases were separated. The aqueous phase was washed with ethyl acetate (2×50 ml). The combined organic phases were dried over magnesium sulphate, filtered and concentrated under vacuum. A yellow oil was obtained which solidified upon storage at room temperature. The solid was triturated with hexane, filtered and dried under vacuum. The title compound was isolated as an off-white solid (4.19 g, 20.9 mmol, 54%).

1. additionadded dropwise to the reaction solution over 2 h at room temperature
2. customthe phases were separated
3. washThe aqueous phase was washed with ethyl acetate (2×50 ml)
4. dry with materialThe combined organic phases were dried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customA yellow oil was obtained which
8. customsolidified upon storage at room temperature
9. customThe solid was triturated with hexane
10. filtrationfiltered
11. customdried under vacuum

ORD record

ord-7cd3c411adac4a7fa21536a15e530d0e

Source dataset

uspto-grants-2006_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07081456B2