(E)-1,3-Dichloropropene → N-(3-Chloro-allyl)-2,2,2-trifluoro-acetamide

Trifluoroacetamide (10.44 g, 92.4 mmol) is dissolved in THF (30 mL). Sodium hydride (60% weight dispersion in mineral oil, 3.1 g, 77 mmol) is then added in small portions at room temperature while regulating the temperature of the reaction with a water bath. The mixture is stirred at room temperature for 5 min., after which E-1,3-dichloropropene (4.5 mL, 49.4 mmol) is added. After 2 min., the mixture thickened, and the reaction was heated to reflux for 45 min. The mixture is then cooled to room temperature, and saturated aqueous ammonium chloride (20 mL) and water (40 mL) are added. The mixture is transferred to a separatory funnel and extracted with ether (2×400 mL). The combined organic layers were dried (MgSO4) and concentrated under reduced pressure to obtained a colorless oil that was used for the next step.

1. customthe temperature of the reaction with a water bath
2. waitAfter 2 min.
3. temperaturethe reaction was heated
4. temperatureto reflux for 45 min
5. temperatureThe mixture is then cooled to room temperature
6. customThe mixture is transferred to a separatory funnel
7. extractionextracted with ether (2×400 mL)
8. dry with materialThe combined organic layers were dried (MgSO4)
9. concentrationconcentrated under reduced pressure
10. customto obtained a colorless oil that

ORDレコード

ord-3992b22bb832446691b93418a66f5dcc

出典データセット

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07741294B1