HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 89561473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 89561451 | HCID 89561451 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 89561473 | HCID 89561473 | 71.2% |
Reaction Steps
To a stirred solution of 2-chloro-N-(3-methylbutyl)-5-nitropyrimidin-4-amine (800 mg, 3.27 mmol) in ethanol (40 ml) was added iron powder (1.8 g). The resulting mixture was heated to reflux before 2 N aqueous hydrochloric acid (4 mL) was added in small portion over 10 min. The reaction was then refluxed for 2 h. The reaction mixture was cooled to rt, filtered to remove inorganic material. The solution was then concentrated under reduced pressure to afforded the desired compound (500 mg), which was used for next step without any further purifications. 1H NMR (CDCl3, 300 MHz) δ 0.92 (d, J=6.8 Hz, 6H), 1.42-1.80 (m, 3H), 3.42-3.60 (m, 2H), 5.01-5.15 (br s 1H), 7.60 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09351974B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-38f266c459624a25aa67ec9fb064d18a |
| Source note | uspto-grants-2016_05 |