HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 6-Bromo-N-methyl-4-nitropyridin-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | 2-Bromo-5-(methylamino)-4-nitropyridine 1-oxide | HCID 86659129 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 6-Bromo-N-methyl-4-nitropyridin-3-amine | HCID 86659130 | — |
Reaction Steps
2-Bromo-5-(methylamino)-4-nitropyridine 1-oxide (10.0 g, 40.4 mmol) in 200 mL dichloromethane was mixed with phosphorous tribromide (10 mL, 106 mmol) in 50 mL dichloromethane at 10° C. and stirred for 10 minutes at ambient temperature. Water and methanol were added and the mixture was extracted with dichloromethane. The organic layers were washed with Na2CO3 (aq.) dried over MgSO4. The residue was triturated with ethanol, filtered and dried at 50° C. i. vac.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598190B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-61cf86ea9cbb4b66b0127a2a0d12e471 |
| Source note | uspto-grants-2013_12 |