HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Thiophenesulfonyl chloride → HCID 21800746, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Thiophenesulfonyl chloride | HCID 85518 | — |
| Reactant | 3-(5-amino-4-chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione | HCID 18619257 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 21800746 | HCID 21800746 | 65.4% |
Reaction Steps
In 5 ml of pyridine was dissolved 0.32 g of 3-(5-amino-4-chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione, and then 0.19 g of 2-thiophensulfonyl chloride was added to the solution at 5 ° C. or lower. Thereafter, the temperature was increased to room temperature and the reaction was continued overnight. Then, pyridine was removed by distillation and the residue was dissolved in ethyl acetate. The solution was washed successively with water, diluted hydrochloric acid and a saturated saline solution, and dried over anhydrous sodium sulfate followed by removing ethyl acetate by distillation to obtain a crude product. This was washed with diisopropyl ether to obtain 0.3 g of the desired compound as white crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05356863 |
| Source dataset | uspto-grants-1994_10 |
| ORD ID | ord-9dc09397e25248288ebffd5f3430f596 |
| Source note | uspto-grants-1994_10 |