HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylhydrazine sulfate → 1-Methyl-5-(trifluoromethyl)-1H-pyrazol-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylhydrazine sulfate | HCID 165286 | — |
| Reactant | 4-Amino-4-ethoxy-1,1,1-trifluorobut-3-en-2-one | HCID 15111754 | — |
| Product | 1-Methyl-5-(trifluoromethyl)-1H-pyrazol-3-amine | HCID 22912798 | 23.1% |
Reaction Steps
Using the procedure described in Example 161A Step 3, (E)-4-amino-4-ethoxy-1,1,1-trifluorobut-3-en-2-one (1.83 g, 10 mmol) and methylhydrazine sulfate (1.586 g, 11 mmol) were reacted and the crude product purified by silica gel chromatography (with 0-10% EtOAc/CH2Cl2 as eluants) to afford 1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-amine as solid (0.381 g, 23%). 1H NMR (300 MHz, CDCl3) δ 5.94 (s, 1H), 3.78 (s, 3H), 3.67 (br, 2H); LC-MS (ESI) m/z 166 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09320739B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-b7e59d1a81344a26af4f10a1353fbf60 |
| Source note | uspto-grants-2016_04 |