HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetyl chloride → HCID 22887946, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 5-Amino-1,2,4-thiadiazole | HCID 290274 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22887946 | HCID 22887946 | — |
Reaction Steps
A solution of [1,2,4]-thiadiazol-5-ylamine (3.0 g) in dry dichloromethane (30 mL) under nitrogen at 0° C. was treated with triethylamine (4.6 mL) followed by slow addition of chloroacetyl chloride (2.6 mL). The reaction mixture was allowed to warm up to room temperature. After 2 h, the mixture was partitioned between dichloromethane and water. The phases were separated and the aqueous layer was extracted with dichloromethane (×2). The combined organic layer was washed with brine, dried over sodium sulphate, filtered and concentrated to give the crude product which was purified by silica gel chromatography eluting with 50-75% EtOAc/cyclohexane to give the title compound (1.00 g) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08329729B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-c17ed5e384d3456cbd8f30f616cb8c58 |
| Source note | uspto-grants-2012_12 |