2,4-difluorophenylethylamine 2,4-Difluorophenylacetic acid → 2-(2,4-Difluorophenyl)acetamide

温度

-78 °C

Preparation of 2,4-difluorophenylethylamine 2,4-Difluorophenylacetic acid (5 g, 29 mmol) in thionyl chloride (50 mL) was heated at reflux for 10 min and the excess thionyl chloride removed by distillation. The acid chloride in dichloromethane (10 mL) was added to a cooled (−78° C.) solution of NH3 (20 mL) in dichloromethane (250 mL). Triethylamine (40 mL) was added and the reaction stirred at ambient temperature for 60 min. The solvents were then evaporated and the remaining solid dissolved in diethyl ether (500 mL). The organic solution was washed with 10% HCl (4×100 mL), 1 N NaOH (4×100 mL), dried over anhydrous MgSO4, filtered and concentrated to afford 630 mg (13%) of 2,4-difluorophenylacetamide.

1. temperaturewas heated
2. temperatureat reflux for 10 min
3. customthe excess thionyl chloride removed by distillation
4. additionThe acid chloride in dichloromethane (10 mL) was added to
5. additionTriethylamine (40 mL) was added
6. customThe solvents were then evaporated
7. dissolutionthe remaining solid dissolved in diethyl ether (500 mL)
8. washThe organic solution was washed with 10% HCl (4×100 mL), 1 N NaOH (4×100 mL)
9. dry with materialdried over anhydrous MgSO4
10. filtrationfiltered
11. concentrationconcentrated

ORDレコード

ord-64189cdccc2c4c35b6ada4b983a1beaa

出典データセット

uspto-grants-2006_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07053104B2