HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 15457064, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| Reactant | HCID 15457058 | HCID 15457058 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 15457064 | HCID 15457064 | — |
Reaction Steps
To 25 ml of chloroform, 0.6 g (1.5 mmol) of 3-(4-chloro-5-chlorosulfonyl-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone and 1.8 g (26.7 mmol) of methylamine hydrochloride were added, and 6.0 g (59.4 mmol) of triethylamine was dropwise added thereto under cooling with ice, followed by stirring at room temperature for 2 hours. This reaction solution was poured into water and extracted with chloroform. After washing with water and a 10% citric acid aqueous solution, the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography to obtain 0.4 g (yield:67) of the desired product. Melting point: 150-151° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06265349B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-c9b0937b700e4fc7b2a81c6aacf66802 |
| Source note | uspto-grants-2001_07 |