反应详情

温度

0 °C

To the solution of 3-[3,5-bis-(1-ethylpropoxy)-4-hydroxyphenyl]acrylic acid (30 mg, 0.09 mmol) in DMF (0.2 ml) and Et3N (10 μl), was added 4-aminomethyl-2,6-di-t-butylphenol (23 mg, 0.10 mmol) at 0° C. and was added the solution of BOP (44 mg, 0.10 mmol) in CH2Cl2 (0.6 ml). The solution was stirred for 30 minutes at 0° C. and then was stirred for 2 hours at room temperature. And then CH2Cl2 was evaporated in vacuo and the obtained residue was poured into ice water. The residue was extracted with EtOAc and washed with HCl (aq) and NaHCO3 (aq). And then the water was dried over anhydrous magnesium sulfate and filtered. The obtained filtrate was vacuum concentrated to give the residue, which was purified by column chromatography (EtOAc:Hexane=1:5), yielding 25 mg (50%) of the title compound as a yellow solid.

1. stirringwas stirred for 2 hours at room temperature
2. customAnd then CH2Cl2 was evaporated in vacuo
3. additionthe obtained residue was poured into ice water
4. extractionThe residue was extracted with EtOAc
5. washwashed with HCl (aq) and NaHCO3 (aq)
6. dry with materialAnd then the water was dried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customto give the residue, which
10. customwas purified by column chromatography (EtOAc:Hexane=1:5)