HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Thiosulfate → 2-Acetylamino-5-propionyl-4-trifluoromethyl-benzoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | 2-Acetylamino-5-(1-hydroxy-propyl)-4-trifluoromethyl-benzoic acid methyl ester | HCID 59164458 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Acetylamino-5-propionyl-4-trifluoromethyl-benzoic acid methyl ester | HCID 59164507 | — |
Reaction Steps
A solution of 2-acetylamino-5-(1-hydroxy-propyl)-4-trifluoromethyl-benzoic acid methyl ester (262 mg, 0.82 mmol) in DCM (1.3 mL) was added to a solution of Dess-Martin periodinane (556 mg, 1.31 mmol) in DCM (2.6 mL) and the mixture was stirred for 1 h at r.t. It was then poured into aqueous sodium thiosulfate and this mixture was extracted with EtOAc. The organic phase was then washed twice with aqueous potassium hydrogencarbonate (pH=8), once with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give crude 2-acetylamino-5-propionyl-4-trifluoromethyl-benzoic acid methyl ester as a white solid which was used without further purification in the next step, ESI-MS: m/z 318 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08012988B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-e3528c06ad63482aa793b863a005351c |
| Source note | uspto-grants-2011_09 |