HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58097243, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl bromoacetate | HCID 60984 | — |
| Reactant | HCID 66671817 | HCID 66671817 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58097243 | HCID 58097243 | — |
Reaction Steps
Under argon, 230 mg (0.363 mmol) of the compound from Example 32A were initially charged in 4 ml of DMF, 17 mg (60% pure, 0.435 mmol) of sodium hydride were added a little at a time and the mixture was then stirred at RT for 30 min. A solution of 41 μl (0.435 mmol) of methyl bromoacetate in 1 ml of DMF was then added dropwise, and the resulting solution was stirred at RT overnight. Water was added, and the reaction mixture was extracted three times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried over sodium sulfate and concentrated. The residue was purified by preparative HPLC (Chromasil, water/acetonitrile).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08609686B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-fceab37b0b1f4eec8f9ea6d07f32747b |
| Source note | uspto-grants-2013_12 |