反応 #2275715

反応方程式

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

trifluoroacetic acid

→

desired compound

収率 89.0%

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

収率 89.0%

溶媒

CH2Cl2

反応条件

後処理

1. 1
   濃縮concentrated under reduced pressure
2. 2
   ろ過The solid that remains is collected by filtration
3. 3
   洗浄washed with Et2O

実験手順

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]+.

出典