HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 19605473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 19605444 | HCID 19605444 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 19605473 | HCID 19605473 | 88% |
Reaction Steps
0.078 g (0.00021 mol) of [2-bromo-6-(4-nitrobenzenesulphonyl) -pyridin-4-yl]-methylamine was dissolved in a mixture of 1.5 ml of methanol and 1.5 ml of dioxane, treated with 0.078 g of iron powder and a solution of 0.078 g of NH4Cl in 2.5 ml of water and heated at reflux for 2 hrs. Therafter, the reaction mixture was poured into a mixture of ethyl acetate and water, suction filtered and the organic phase was extracted with water and sat. sodium chloride solution and dried over MgSO4. After removal of the solvent the residue was chromatographed on silical gel with ethyl acetate/hexane 1:3. There was obtained 0.063 g (88%) of [2-(4-aminobenzenesulphonyl)-6-bromopyridin-4-yl]-methylamine as yellowish crystals; m.p.: 158-160° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05990105 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-e14a0a2544fe475fa759e025b6ae2a34 |
| Source note | uspto-grants-1999_11 |