HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine hydrate (1:1) → HCID 22046500, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 22046519 | HCID 22046519 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22046500 | HCID 22046500 | 72.4% |
Reaction Steps
To a stirred solution of 1-[5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-pyrazin-2-yl]-3-(2-methoxy-5-methyl-phenyl)-urea (16 mg, 38 μmol) in 380 μL 95% EtOH and 100 μL DMF at room temperature in a capped reaction vial was added hydrazine monohydrate (3.8 μL, 76 μmol). After stirring overnight at room temperature, a white precipitate formed. The precipitate was filtered off, dried and triturated with EtOAc to remove phthalimide based impurities to provide the product as a white solid (7.9 mg, 72%). 1H-NMR (400 MHz, d6-DMSO) δ 9.54 (s, 1H), 8.80 (s, 1H), 8.46 (s, 1H), 8.02 (s, 1H), 6.93 (d, 1H), 6.79 (d, 1H), 4.51 (d, 2H), 4.39 (br s, 2H), 3.89 (s, 3H), 2.23 (s, 3H). LRLCMS (ESI, Positive) m/e 288.2 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07608618B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-50bb29a9342748efab53b52ba31fac14 |
| Source note | uspto-grants-2009_10 |