反应详情

温度

130 °C

To a solution of 1.5 g (6.9 mmol) of the product of Example 1 in 15 mL of HOAc-H2O (11:3) was added 1.17 g (8.3 mmol) of hexamethylenetetramine dissolved in 3 mL water. The reaction mixture was magnetically stirred and heated at 130° C. for 3 h at which point 13.5 mL of a 2:1 solution of conc. hydrochloric acid and water was added. The reaction mixture was heated for an additional 10 min at 130° C., then cooled to room temperature and the acetic acid was removed on a rotary evaporator. The residue was partitioned between EtOAc and water, then extracted and the organic layers were combined and dried (Na2SO4). The filtrate was passed through a layer of Celite filter aid mixed with silica gel to remove polar impurities, then evaporated. The residual oil was dried in vacuo and subsequently used in the next step without further purification.

1. additionwas added
2. temperatureThe reaction mixture was heated for an additional 10 min at 130° C.
3. temperaturecooled to room temperature
4. customthe acetic acid was removed on a rotary evaporator
5. customThe residue was partitioned between EtOAc and water
6. extractionextracted
7. dry with materialdried (Na2SO4)
8. filtrationfilter aid
9. additionmixed with silica gel
10. customto remove polar impurities
11. customevaporated
12. customThe residual oil was dried in vacuo
13. customsubsequently used in the next step without further purification