HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropylamine → 3-methyl-N-(1-methylethyl)-2-nitrobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropylamine | HCID 6363 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 3-Methyl-2-nitrobenzoic acid | HCID 21575 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-methyl-N-(1-methylethyl)-2-nitrobenzamide | HCID 890272 | 80.2% |
Reaction Steps
A solution of 3-methyl-2-nitrobenzoic acid (2.00 g, 11.0 mmol) and triethylamine (1.22 g, 12.1 mmol) in 25 mL of methylene chloride was cooled to 10° C. Ethyl chloroformate was carefully added and a solid precipitate formed. After stirring for 30 minutes isopropylamine (0.94 g, 16.0 mmol) was added and a homogeneous solution resulted. The reaction was stirred for an additional hour, poured into water and extracted with ethyl acetate. The organic extracts were washed with water, dried over magnesium sulfate and evaporated under reduced pressure to afford 1.96 g of the desired intermediate as a white solid melting at 126-128° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696232B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-bd1de19a5f4042cc93bad23b36ddefed |
| Source note | uspto-grants-2010_04 |