HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 58574195, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Hexamethyldisilazane | HCID 13838 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | HCID 69937721 | HCID 69937721 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58574195 | HCID 58574195 | — |
Reaction Steps
The mixture of tert-butyl 2-(5-bromo-2-(methylcarbamoyl)phenylcarbamoyl)pyrrolidine-1-carboxylate (0.2 g, 0.47 mmol), hexamethyldisilazane (0.39 mL, 1.88 mmol), I2 (0.24 g, 0.94 mmol), and DCM (10 mL) was refluxed for 5 h under nitrogen atmosphere. Na2S2O3 aqueous solution was added to quench the reaction followed by cooling to room temperature. The organic layer was separated and the water layer was extracted with ethyl acetate (3×10 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered, and evaporated to give the desired product, which was directly used for the next step. MS (ESI): 308, 310 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772301B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-38bbbf828ad84c22a2a663bbb3a8cd91 |
| Source note | uspto-grants-2014_07 |