HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Phosphate, Dibasic → HCID 22125638, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Phosphate, Dibasic | HCID 24450 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | 2-Amino-5-bromo-1,3,4-thiadiazole | HCID 3650883 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22125638 | HCID 22125638 | 56.6% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A mixture of 5-bromo-1,3,4-thiadiazol-2-ylamine (9.27 g), Boc-piperazine (11.51 g), and K2HPO4 (13.4 g) in 30 ml of DMF is heated at 100° C. under argon for four hours, then cooled and added to 100 g of ice. The mixture is extracted with ethyl acetate, and the organic phase washed twice with water and dried (MgSO4). Following removal of the solvent under reduced pressure, the residue is flash chromatographed on silica using 4% methanol in dichloromethane to afford 8.32 g of the title compound as a solid. Recrystallization from 240 ml of 1:1 acetonitrile-toluene provides 6.65 g of solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06150385 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-193de3cff80b4363b0153423c96924f6 |
| Source note | uspto-grants-2000_11 |