HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]benzenesulfonyl chloride → 3-(4-Chloro-2-fluoro-5-sulfanylphenyl)-1-methyl-6-(trifluoromethyl)-1,2,3,4-tetrahydropyrimidine-2,4-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]benzenesulfonyl chloride | HCID 15334535 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 3-(4-Chloro-2-fluoro-5-sulfanylphenyl)-1-methyl-6-(trifluoromethyl)-1,2,3,4-tetrahydropyrimidine-2,4-dione | HCID 18619270 | 97.1% |
Reaction Steps
1.65 g of 2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]benzenesulfonyl chloride was dissolved in 16 ml of acetic acid, to this was added 4.4 g of zinc, then, they were reacted while heating under reflux. After completion of the reaction, the reaction solution was cooled, then, this was poured into ice water, extracted with ethyl acetate, and filtrated. The filtrate was separated, then, the organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated to obtain 1.35 g of 2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenyl mercaptan.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06537948B1 |
| Source dataset | uspto-grants-2003_03 |
| ORD ID | ord-a4e3156ef4284f35b3572c0c4ceae3fa |
| Source note | uspto-grants-2003_03 |