HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 9821271, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Fluorobenzyl bromide | HCID 68021 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 15486861 | HCID 15486861 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 9821271 | HCID 9821271 | 53% |
Reaction Steps
To a solution of the compound obtained in Example 5 (4) (2.3 mg) in N,N-dimethylformamide (0.5 ml), 60% sodium hydride (0.5 mg) was added at 0° C. and the mixture was stirred at the same temperature for 15 minutes. p-Fluorobenzyl bromide (2.4 mg) was then added thereto at 0° C. and the mixture was stirred at 15 to 30° C. for 1 hour. The reaction solution was poured into a saturated aqueous sodium hydrogencarbonate solution, extracted with toluene, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was separated using silica gel preparative thin-layer chromatography (chloroform:methanol=100:1) to obtain 1.7 mg of the desired product as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06875770B2 |
| Source dataset | uspto-grants-2005_04 |
| ORD ID | ord-72faf2e761c34f2aa40071b60b7d6b58 |
| Source note | uspto-grants-2005_04 |