反应详情

温度

0 °C

20 mmol of 4-Amino-3-hydroxymethyl-benzonitrile were dissolved in THF. 1.2 eq. of DIPEA were added and the reaction cooled to 0° C. 3.5 eq of ethyl chloroformate were added dropwise and the reaction warmed to rt and stirred for another 15 min. The crude material was extracted form etyhlacetate and sat. NaHCO3. After separation, and drying of the organic layer the solvent was evaporated and the crude taken up in toluene. 2.5 ml of DBU were added and the reaction mixture refluxed for 4 h. The organic layer was extracted with water and the organic layer separated and reduced resulting in a yellow oil. Crude material was not further characterized.

1. temperaturethe reaction warmed to rt
2. extractionThe crude material was extracted form etyhlacetate and sat. NaHCO3
3. customAfter separation
4. customdrying of the organic layer the solvent
5. customwas evaporated
6. addition2.5 ml of DBU were added
7. temperaturethe reaction mixture refluxed for 4 h
8. extractionThe organic layer was extracted with water
9. customthe organic layer separated
10. customreduced resulting in a yellow oil