HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → 4-Benzothiazol-2-YL-N3-(2-ethylaminoethyl)-1H-pyrazole-3,5-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | N-[2-(5-amino-4-benzothiazol-2-yl-1H-pyrazol-3-ylamino)ethyl]acetamide | HCID 66768089 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-Benzothiazol-2-YL-N3-(2-ethylaminoethyl)-1H-pyrazole-3,5-diamine | HCID 66768004 | — |
Reaction Steps
N-[2-(5-Amino-4-benzothiazol-2-yl-1H-pyrazol-3-ylamino)ethyl]acetamide (80 mg, 0.25 mmol) and lithium aluminum hydride (92 mg) were refluxed in anhydrous THF (10 mL) for 3 hrs. The resulting mixture was poured into a saturated ammonium chloride solution (50 mL). The aqueous phase was extracted with ethyl acetate (3×50 mL). The combined extracts were washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated to yield 54 mg of crude product. The crude product was purified by flash column chromatography eluting with CH2Cl2:MeOH=5:1 with 0.5% NH3. The title compound was isolated in a yield of 36 mg (48%). MS (m/z, ES+): 303.1 (M+1, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410272B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-d8f366d899604dcda184d275b0e2b7a0 |
| Source note | uspto-grants-2013_04 |