HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodoethane → HCID 66997992, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodoethane | HCID 6340 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 66738218 | HCID 66738218 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66997992 | HCID 66997992 | 101.5% |
Reaction Steps
Add sodium hydride (84.0 mg, 2.1 mmol, 60% dispersion in mineral oil) to a solution of [1-(6-fluoro-4-iodo-pyridin-3-yl)-ethyl]-carbamic acid tert-butyl ester (0.37 g, 1.0 mmol) in dimethylformamide (10 mL). Stir at room temperature for 30 min. Add iodoethane (0.2 mL, 2.1 mmol). Stir for 1 hour. Quench the reaction with water. Extract with CH2Cl2. Wash the organic layer with water and saturated aqueous sodium chloride. Dry over MgSO4. After filtration, afford crude product ethyl-[1-(6-fluoro-4-iodo-pyridin-3-yl)-ethyl]-carbamic acid tert-butyl ester (0.4 g, 97%) with 90% HPLC purity, MS (ES) m/z 395 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063212B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-67baa8792da747eda85c8fc0a371ec05 |
| Source note | uspto-grants-2011_11 |