反应详情

温度

0 °C

A suspension of 5-(2,4-bis-benzyloxy-5-chloro-phenyl)-isoxazole-3-carboxylic acid ethylamide (1 g, 2.2 mmol) in Ac2O (20 ml) was cooled to 0° C. and HNO3 (0.26 ml, 4.3 mmol) was added dropwise under stirring, the temperature being maintained between 0-5° C. After the addition was complete, the mixture was stirred for 70 h at 5-10° C. and then poured into ice and extracted with DCM (3×40 ml). The extract was dried and concentrated under vacuo. The yellow solid obtained was triturated with Et2O and filtered to give 5-[2,4-bis(benzyloxy)-5-chlorophenyl]-N-ethyl-4-nitroisoxazole-3-carboxamide (810 mg, 73%).

1. temperaturethe temperature being maintained between 0-5° C
2. additionAfter the addition
3. stirringthe mixture was stirred for 70 h at 5-10° C.
4. additionpoured into ice
5. extractionextracted with DCM (3×40 ml)
6. customThe extract was dried
7. concentrationconcentrated under vacuo
8. customThe yellow solid obtained
9. customwas triturated with Et2O
10. filtrationfiltered