반응 #2275715

반응 방정식

[(3,5-dihydroxy-pyridine-2-carbonyl)-amino]-acetic acid tert-butyl ester

trifluoroacetic acid

→

desired compound

수율 89.0%

[(3,5-dihydroxy-pyridine-2-carbonyl)-amino]-acetic acid

수율 89.0%

용매

CH2Cl2

반응 조건

후처리

1. 1
   농축concentrated under reduced pressure
2. 2
   여과The solid that remains is collected by filtration
3. 3
   세척washed with Et2O

실험 절차

To a solution of [(3,5-dihydroxy-pyridine-2-carbonyl)-amino]-acetic acid tert-butyl ester, 28, (0.10 g, 0.37 mmol) in CH2Cl2 (4 mL) at room temperature is added trifluoroacetic acid (1 mL). The reaction is stirred for 16 hours at room temperature and then concentrated under reduced pressure. The solid that remains is collected by filtration, washed with Et2O to afford 0.070 g (89% yield) of the desired compound as a colorless solid. 1H NMR (250 MHz, DMSO-d6) δ ppm 10.86 (1H, br s), 9.00 (1H, t, J=6.1 Hz), 7.77 (1H, d, J=2.4 Hz), 6.69 (1H, d, J=2.4 Hz), 3.95 (1H, d, J=6.2 Hz). HPLC-MS: m/z 213 [M+H]+.

출처