![]() ![]() This extraction was repeated, and the original decantation and the second extract combined and filtered to remove a few hundred milligrams of unwanted solids. ![]() The dry solids were transferred to a beaker, suspended in 50 mL 15% ammonia in anhydrous ethanol, stirred for 1 h, and separated by decantation. The reaction mixture was cooled overnight, the solids removed by filtration, and the filter cake washed with 10 mL Et 2O. White solids started to appear early in the neutralization approximately 60 mL of sulfuric acid was required. The reaction mixture was cooled to about 10 ☌ with an external ice bath, and acidified to a pH of about 3.0 by the dropwise addition of 2.5 N H 2SO 4. The stirring was continued for an additional 3 h. The reaction mixture turned yellow as the ergotamine went into solution over the course of 1 h. ![]() SYNTHESIS: A solution of 6.7 g KOH in 100 mL H 2O, under an inert atmosphere and magnetically stirred, was brought to 75 ☌, and 10 g ergotamine tartrate (ET) added. ![]()
0 Comments
Leave a Reply. |
AuthorWrite something about yourself. No need to be fancy, just an overview. ArchivesCategories |