Hydrochloric Acid → HCID 54329319, compound

Triphenylphosphine (873 mg) was added to a solution of 2-(1-azidoethyl)-5-fluorothiophene (518 mg) in THF (10 mL), and the reaction solution was stirred at room temperature for 1 hour. Water (2 mL) was added to the reaction mixture, and the mixture was heated to reflux for 3 hours. After allowing the reaction mixture to be cooled, a 5 N aqueous solution of hydrochloric acid and ethyl acetate were added thereto to separate the aqueous layer. A 5 N aqueous solution of sodium hydroxide was added to the aqueous layer to make the layer basic, and the aqueous layer was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 324 mg of the title compound. The physical properties of the compound are as follows.

1. temperaturethe mixture was heated
2. temperatureto reflux for 3 hours
3. temperatureto be cooled
4. customto separate the aqueous layer
5. additionA 5 N aqueous solution of sodium hydroxide was added to the aqueous layer
6. extractionthe aqueous layer was extracted with ethyl acetate
7. washThe organic layer was washed with brine
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated under reduced pressure

ORD record

ord-bcf772a1b10f4ba18905f68b82dcb43e

Source dataset

uspto-grants-2010_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07687640B2