HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 58522649, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Ethyl 2-acetyl-6-nitrobenzoate | HCID 53434730 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Product | HCID 58522649 | HCID 58522649 | — |
Reaction Steps
Ethyl-2-acetyl-6-nitrobenzoate (11.12 g) is suspended in a mixture of MeOH (70 mL) and MgSO4. Methylamine (2 molar in THF, 28.13 mL) is added dropwise and the solution is stirred for 15 min at this temperature. Then it is preheated to 70° C. for 18 h. The solvent is eliminated in vacuo, the residue is taken up in dichloromethane (100 mL), washed with sodium chloride solution (10%) dried on magnesium sulphate, filtered off from the desiccant and the solvent is eliminated in vacuo. For purification it is recrystallised from toluene (250 mL).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846689B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-bf2e1c2a43e14672afa57ac8c6f817de |
| Source note | uspto-grants-2014_09 |