HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Methoxide → HCID 66701012, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | Ethyl 5-fluoro-2-sulfanylbenzoate | HCID 16217758 | — |
| Reactant | HCID 43700001 | HCID 43700001 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 66701012 | HCID 66701012 | 70.7% |
Reaction Steps
To a solution of 1.00 g 5-fluoro-2-mercaptobenzoic acid ethyl ester in 10 ml methanol 0.81 g of sodium methoxide were added portionwise, followed by addition of 0.97 g 2-(2-chloro-acetylamino)-2-methyl-propionic acid methyl ester. After refluxing the reaction under argon-atmosphere for 0.5 h the resulting mixture was filtrated, 20 ml water and 1.25 ml of acetic acid were added and the precipitated product was collected by filtration, washed with water, dissolved in ethyl acetate and THF, dried over sodium sulphate, filtrated and concentrated in vacuo. The resulting crude product was crystallized from diethylether to yield 1.10 g 2-[(5-fluoro-3-hydroxy-benzo[b]thio-phene-2-carbonyl)-amino]-2-methyl-propionic acid methyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08283479B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-a79b41356cf04122be7460093b5b2929 |
| Source note | uspto-grants-2012_10 |