HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 82115337, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 3-Chloro-2-methylaniline | HCID 6894 | — |
| Reactant | Methyl 3-bromopropanoate | HCID 76934 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Hexamethylphosphoramide | HCID 12679 | — |
| Product | HCID 82115337 | HCID 82115337 | 57.2% |
Reaction Steps
1.00 g of 3-chloro-2-methylaniline was dissolved in 10 mL of hexamethylphosphoramide, and 1.80 g of sodium hydrogen carbonate and 1.19 g of methyl 3-bromopropionate sequentially were added thereto, followed by stirring at room temperature for 4 hours. To the reaction liquid was added water, followed by extraction with diisopropyl ether. The organic layer was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=95:5 to 85:25) to obtain 0.92 g of methyl N-(3-chloro-2-methylphenyl)-β-alanine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973078B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-eb07c74021454c2b9a8bbaa981dbc09c |
| Source note | uspto-grants-2011_07 |