HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22902325, compound → HCID 22902365, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22902325 | HCID 22902325 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22902365 | HCID 22902365 | 56.6% |
Reaction Steps
2.1 g of 3-(3-[N-(2-(4-nitrophenyl)-ethyl)-N-methylamino]-propyloxy)-5-phenyl-1,2,4-thiadiazole (for) preparation, see Example 8)), were dissolved in a mixture of 75 ml ethanol and 75 ml methanol and reacted with a catalytic quantity of Raney nickel. The reaction mixture was then hydrogenated for 2.5 hours at room temperature with hydrogen at a hydrogen pressure of 5 bars. The catalyst was filtered off and the filtrate concentrated to dryness. The oily crude title compound obtained was purified by medium-pressure chromatography over fine-grained silica gel (Lichroprep Si 60®) using 95:5 ethyl acetate/methanol as the eluent. 1.1 g of the title compound were obtained as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05547967 |
| Source dataset | uspto-grants-1996_08 |
| ORD ID | ord-e44059025aa8415e924a50359a67e5cb |
| Source note | uspto-grants-1996_08 |