Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine hydrochloride | HCID 11130 | — |
| Reactant | Dimethylacetamide | HCID 31374 | — |
| Reactant | HCID 15100939 | HCID 15100939 | — |
| Reactant | Sodium bicarbonate water | HCID 86585896 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 2866-68-4 | HCID 11138325 | — |
Reaction Steps
In 3-(4-chlorobenzyl)-2-oxocyclopentane carboxylic acid methyl ester (1.0 g, 0.00375 mol), N,N-dimethylacetamide (1 mL) and triethylamine hydrochloride (0.774 g, 0.00375×1.5 mol) were added and stirred at 130° C. for 2 hours, and then at 140° C. for another 3 hours. In the reaction liquid, ethyl acetate and saturated sodium bicarbonate water were added, and the mixture was partitioned. After extracting the aqueous layer using ethyl acetate, the organic layer was dried using anhydrous sodium sulfate and concentrated. Thereafter, the dried and concentrated product was purified using a silica gel column, and a target product was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09206106B2 |
|---|
| Source dataset | uspto-grants-2015_12 |
|---|
| ORD ID | ord-4fd196e6f7204210b74c6370839edbe8 |
|---|
| Source note | uspto-grants-2015_12 |
|---|