HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 57675165, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 57675182 | HCID 57675182 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57675165 | HCID 57675165 | — |
Reaction Steps
A solution of Intermediate 120 (46 mg, 0.1 mmol) in dry dimethylformamide (2 ml) was added to sodium hydride (60% dispersion in mineral oil, 4.4 mg, 0.11 mmol), and the resulting mixture was stirred at room temperature. After 16 h, the reaction mixture was diluted with water (2 ml) and extracted with chloroform (3×5 ml). The combined organic extracts were dried over anhydrous sodium sulphate and evaporated to give the crude product. Purification of the crude product on a SPE cartridge (silica, 2 g) using a gradient of ethyl acetate in petroleum ether afforded Example 174. LCMS showed MH+=426, TRET=2.66 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07528148B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-b1005866eb4b410b87a366074ed0eae6 |
| Source note | uspto-grants-2009_05 |