HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 53822792, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | 1-Propanesulfonyl chloride | HCID 66279 | — |
| Reactant | N-Nitro-S-methylisothiourea | HCID 135927615 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 53822792 | HCID 53822792 | 60.5% |
Reaction Steps
A mixture of S-methyl-N-nitroisothiourea (5.0 g), CH3CN (50 ml) and Et3N (11.2 g) was cooled with iced water. To the cooled mixture was added 10.6 g of n-propanesulfonyl chloride dropwise below 15° C. under stirring. After stirring at the same temperature for 1 hour, the mixture was poured into a mixed solution of conc. hydrochloric acid (20 ml) and water (180 ml) and the resulting mixture was extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated in vacuo to afford 9.9 g of crude crystals. Recrystallization of the product from CCl4 (5 ml) gave 5.4 g of S-methyl-N-nitro-N'-(n-propanesulfonyl)isothiourea as a pale yellow crystal, m.p. 91°-93° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05256679 |
| Source dataset | uspto-grants-1993_10 |
| ORD ID | ord-f698fffb73f248b3ada9feab17a7c6d8 |
| Source note | uspto-grants-1993_10 |