Triphenylphosphine → HCID 71601674, compound

Temperature

45 °C

Compound 27c (4.8 g, 20 mmol) was dissolved in tetrahydrofuran (10 mL). Under the protection of argon, PPh3 (5.8 g, 22 mmol) was added, and the reaction mixture was heated to 45° C. to react for 2 hrs. Then water (7.86 mL) was added and the mixture was cooled to room temperature to react for 13 hrs. TLC (dichloromethane/methanol=20/1) was employed to monitor the reaction. After the reaction completed, the mixture was diluted with water, and extracted with ethyl acetate. The organic phase was combined, washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate, and then dried by rotary evaporation. Column chromatography afforded 4.0 g of white solid (compound 27d), yield 93.2%.

1. customto react for 2 hrs
2. temperaturethe mixture was cooled to room temperature
3. customto react for 13 hrs
4. customthe reaction
5. extractionextracted with ethyl acetate
6. washwashed with saturated sodium chloride solution
7. dry with materialdried over anhydrous sodium sulfate
8. customdried by rotary evaporation

ORD record

ord-bc46325822c84a9bad750e746ff2c551

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09416144B2