HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (2R,4R)-2-[2-Fluoro-4-(3-methyl-pyrazol-1-yl)-phenylcarbamoyl]-4-methoxy-pyrrolidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Ethoxy-1-(ethoxycarbonyl)-1,2-dihydroquinoline | HCID 27833 | — |
| Reactant | (2R,4R)-1-[(tert-butoxy)carbonyl]-4-methoxypyrrolidine-2-carboxylic acid | HCID 11459222 | — |
| Reactant | 2-Fluro-4-(3-methyl-pyrazol-1-yl)phenylamine | HCID 22181526 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | (2R,4R)-2-[2-Fluoro-4-(3-methyl-pyrazol-1-yl)-phenylcarbamoyl]-4-methoxy-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 68805326 | — |
Reaction Steps
(2R,4R)-4-methoxy-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester (0.350 g, 1.427 mmol), aniline 1 (0.273 g, 1.427 mmol) and EEDQ (0.529 g, 2.140 mmol) were dissolved in CHCl3 (30 mL). Et3N (0.6 mL, 4.281 mmol) was added and the reaction mixture was heated at reflux for 18 h. The mixture was allowed to cool and diluted with CHCl3 (100 mL) and washed with 5% HCl, 0.5 N NaOH, water and brine (40 mL each), the organic extract was dried over MgSO4, filtered and the solvent removed to give a pale tan foam. The crude product was used for the next step without purification. MS: APCI (AP+): 419.2 (M)+, (AP−): 417.2 (M)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07407972B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-7b47025a36b146cb81354a41d1e3c5b5 |
| Source note | uspto-grants-2008_08 |