HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 58137436, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | HCID 57943993 | HCID 57943993 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58137436 | HCID 58137436 | — |
Reaction Steps
5-Amino-2-methyl-4-(pentafluorosulfanyl)benzoic acid (500 mg, WO 2005/47239) was dissolved in methylene chloride (30 ml) and admixed while stirring with N,O-dimethylhydroxylamine hydrochloride (176 mg), 1-propanephosphonic anhydride (1.1 ml) and triethylamine (0.25 ml). After stirring for 4 h and leaving to stand overnight, the reaction mixture was concentrated, the residue was taken up with ethyl acetate and the solution was washed twice with potassium hydrogen sulfate solution and twice with sodium hydrogencarbonate solution. After drying over magnesium sulfate, the organic phase was filtered and concentrated. The resulting crude product (500 mg) was converted further directly.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08466169B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-532dcba4d0f84bf19d01c07b40f804e5 |
| Source note | uspto-grants-2013_06 |