HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiophenol → HCID 86738000, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 86738001 | HCID 86738001 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86738000 | HCID 86738000 | 45% |
Reaction Steps
A solution of 24.5 ml of thiophenol in 100 ml of anhydrous THF is added to a suspension of 13 g of sodium methylate in 440 ml of absolute THF whilst stirring at room temperature under nitrogen. 72 g of 4-chloro-3-nitro-5-pyrrol-1-yl-sulfonylbenzoic acid methyl ester in 220 ml of absolute THF are then added dropwise and the mixture is stirred at room temperature until the end of the reaction is reached, as ascertained by thin layer chromatography. After removing the solvent on a rotary evaporator, the residue is repeatedly extracted with hexane and then recrystallized from ethyl acetate/methanol. 3-Nitro-4-phenylthio-5-pyrrol-1-yl-sulfonyl-benzoic acid methyl ester of melting point 153°-154° C. is obtained. Yield: 45%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04288449 |
| Source dataset | uspto-grants-1981_09 |
| ORD ID | ord-dc2b80f07c0049bea5b16f16e365968f |
| Source note | uspto-grants-1981_09 |