Triethylamine → (E)-Ethyl 3-(2-amino-5-(trifluoromethyl)phenyl)acrylate

温度

120 °C

To a mixture of 2-bromo-4-(trifluoromethyl)aniline (5 g, 20.83 mmol), triethylamine (4.4 mL, 31.2 mmol) and P(o-tol)3 (2.5 g, 8.33 mmol) in DMF (42 mL, 0.5 M) in a glass pressure tube under nitrogen gas were added ethyl acrylate (2.3 g, 23 mmol) and palladium acetate (940 mg, 4.167 mmol). The tube was sealed and heated to 120° C. for 18 h. The resulting solution was concentrated under vacuum and purified by column chromatography. Retention time(min)=2.532, method [1], MS(ESI) 260.1 (M+H).

1. customThe tube was sealed
2. concentrationThe resulting solution was concentrated under vacuum
3. custompurified by column chromatography

ORDレコード

ord-8afb3c3aa796465d9d6a3ac373f0ba41

出典データセット

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09073891B2