HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 23323065, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | Tetrafluoro-m-phenylenediamine dihydrochloride | HCID 149026 | — |
| Reactant | 5-[(4-Methyl-8-nitroquinolin-6-yl)methyl]pyrimidine-2,4-diamine | HCID 23323050 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | 2-Methoxyethanol | HCID 8019 | — |
| Product | HCID 23323065 | HCID 23323065 | 69% |
Reaction Steps
The product of Example 12 (0.78 g, 2.5 mmol) was dissolved in 35 ml of β-methoxyethanol, and then 0.06 g of 5% Pd/C and 0.3 ml of 95% hydrazine were added, and the reation was refluxed for 1 hour. The Pd/C was filtered off, the solvent removed, and the product was purified on a silica gel column which was eluted with 7% methanol in methylene chloride. This gave 0.48 g (69% yield) of the free base which was recrystallised as the dihydrochloride salt from ethanol, mp 303°-305° dec. Anal. Calcd. for C15H16N6.2HCl.0.5H2O: C, 49.73; H, 5.29; N, 23.20; Cl, 19.57. Found: C, 49.71; H, 5.30; N, 23.18; Cl, 19.51.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04587341 |
| Source dataset | uspto-grants-1986_05 |
| ORD ID | ord-7f0e4980e40b43c3972eabb37bab6ff6 |
| Source note | uspto-grants-1986_05 |