反应详情

A mixture of the gummy triester (5)(0.633 g, 0.001 mole), H2O (18 mL), EtOH (18 mL), and 1.00N NaOHaq (5 mL, 0.005 mole) was placed in a conical flask and stirred vigorously (magnetic stirrer) for 40 minutes to give a pale yellow solution. This solution was kept at 22° C. for 18.5 hours. It was then filtered through a bed of Celite (carbon treatment) and the clear filtrate acidified to pH 2.5 with 1.00 N HClaq. The resulting white gelatinous precipitate of the product was centrifuged (1500g/30 minutes) and washed by three cycles of resuspension (H2 0: 80 mL, 80 mL, and 40 mL)--centrifugation--decantation. The pellet was dried in vacuo over P2 05 --first at 22° C./24 hours in a desiccator and then at 80° C./4 hours in a pistol. A pale yellow amorphous solid was obtained (0.312 g, 67.5%),

1. customwas placed in a conical flask
2. customto give a pale yellow solution
3. waitThis solution was kept at 22° C. for 18.5 hours
4. filtrationIt was then filtered through a bed of Celite (carbon treatment)
5. custom(1500g/30 minutes)
6. washwashed by three cycles of resuspension (H2 0: 80 mL, 80 mL, and 40 mL)
7. customThe pellet was dried in vacuo over P2 05
8. customat 22° C.
9. custom24 hours
10. customat 80° C.
11. custom4 hours
12. customA pale yellow amorphous solid was obtained (0.312 g, 67.5%)