反应详情

To a solution of 5-benzyloxy-2-[1-(4-chlorophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid tert-butyl ester (323) (4.82 g, 9.74 mmol) in tetrahydrofuran (90 mL) and water (45 mL) was added LiOH.H2O (4.086 g, 97.37 mmol). The reaction mixture was heated to reflux for 20 h (the reaction was monitored by LC-MS). The tetrahydrofuran was removed in vacuo and the reaction mixture was diluted with water (100 mL) and extracted with ethyl acetate (2×50 mL). The aqueous layer was acidified with 1N HCl to about pH 3. A white solid was separated by filtration and dried in vacuo to get pure 5-benzyloxy-2-[1-(4-chlorophenyl)-cyclopentylmethyl]-6-hydroxypyrimidine-4-carboxylic acid (324) (3.47 g, 81%).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 20 h (the reaction
3. customThe tetrahydrofuran was removed in vacuo
4. additionthe reaction mixture was diluted with water (100 mL)
5. extractionextracted with ethyl acetate (2×50 mL)
6. customA white solid was separated by filtration
7. customdried in vacuo