HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thioglycerol → HCID 178472730, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thioglycerol | HCID 7291 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 178472731 | HCID 178472731 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178472730 | HCID 178472730 | 30% |
Reaction Steps
To a solution of compound G (5.5 g, 6.5 mmol) in DMF (21 mL) at ambient temperature was added K2CO3 (8.9 g, 64.5 mmol) followed by thioglycerol (5.6 mL, 64.5 mmol). The reaction mixture was stirred at ambient temperature for 1 h, filtered off and DMF was removed in vacuo. The residue was diluted with water (500 mL) and extracted with EtOAc (2×300 mL) and CHCl3 (2×300 mL). Combined organic layers were dried and removal of the solvents in vacuo afforded the crude product. The crude product was purified by flash chromatography eluting with EtOAc followed by 10% MeOH in CHCl3 to afford compound H (1.3 g, 30%). LC-MS [M+H] 668.3 (C30H49N7O8S+H, calc: 667.8). Purity >95% (UV/254 nm).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040032B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-cd87975301a8442bbaf3d3d6986f2e11 |
| Source note | uspto-grants-2015_05 |