HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 21156212, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 21156211 | HCID 21156211 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21156212 | HCID 21156212 | — |
Reaction Steps
A solution of 6 g of 1-(t-butyl)-9,10-didehydro-6-methyl-8β-hydroxymethyl-ergoline, prepared as described in Example 1, in 500 ml of methanol and 5 ml of sulphuric acid was irradiated at 20° C. in a Pyrex flask with a Hanau PL 321 lamp for about 6 hours, until the absorption at 315 nm completely disappeared. The solution was diluted with iced water, made basic with ammonium hydroxide, evaporated to 100 ml and extracted with ethyl acetate. After evaporation of the solvent the residue was chromatographed in silica gel and on elution with 97:3 dichloromethane:methanol, 5 g of the title compound was isolated, m.p. 172 to 174° C. from acetone.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05079364 |
| Source dataset | uspto-grants-1992_01 |
| ORD ID | ord-3734648caf0b49cea12e194d662dcbe6 |
| Source note | uspto-grants-1992_01 |