HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine, hydrochloride → HCID 66909141, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 2-Chloro-4-fluorobenzoate | HCID 2763551 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 66909141 | HCID 66909141 | 99% |
Reaction Steps
To a stirred solution of 4.00 g (20.6 mmol) 2-chloro-4-fluoro-benzoic acid methyl ester (Apollo) and 60 ml dimethylsulphoxid were added 2.03 g (24.7 mmol) dimethylamine hydrochloride and 5.97 g (43.2 mmol) potassium carbonate. The reaction mixture was stirred over night and is reduced with high vacuum rotation evaporator at 65° C. The residue was diluted with dichloromethane, washed twice with water. The combined water phases were extracted with dichloromethane. The combined dichloromethane phases were washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The oily crude product 1a was obtained in 99% yield (4.36 g, 20.4 mmol) and was used for the next step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557776B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-084458ee25ef456180111f08904daea6 |
| Source note | uspto-grants-2013_10 |