HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid monohydrate → HCID 19704095, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 19703789 | HCID 19703789 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 19704095 | HCID 19704095 | 13.2% |
Reaction Steps
A solution of N-[[(4-cyano-2-thiazolyl)amino]thioxomethyl]-DL-phenylalanine methyl ester (1.42 g, 4.10 mmol) and p-toluene sulfonic acid hydrate (0.20 g 1.05 mmol) in toluene (80 mL) was refluxed with a Dean-Stark trap for 24 h. The reaction was cooled to room temperature, solvent removed under reduced pressure, residue taken up in ethyl acetate, washed with saturated sodium bicarbonate and saturated sodium chloride, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting product was recrystallized from ethyl ether-hexanes to provide 170.1 mg (10%) of the titled product:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05593993 |
| Source dataset | uspto-grants-1997_01 |
| ORD ID | ord-ceac218dc4844826996bc2f00c4ebaf4 |
| Source note | uspto-grants-1997_01 |