HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 22504428, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4-Fluorobenzyl bromide | HCID 68021 | — |
| Reactant | HCID 22504411 | HCID 22504411 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22504428 | HCID 22504428 | 99.6% |
Reaction Steps
To a solution of the compound obtained in Example 34 (5) (10 mg) in N,N-dimethylformamide (0.5 ml), 60% sodium hydride (3 mg) was added at 0° C. and the mixture was stirred for 20 minutes. To the resulting mixture was added dropwise 4-fluorobenzyl bromide (15 mg) and the mixture was stirred at 15 to 30° C. for 30 minutes. The reaction solution was poured into a saturated aqueous ammonium chloride solution, extracted with chloroform, washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The resulting residue was separated using silica gel preparative thin-layer chromatography (hexane:ethyl acetate=5:1) to obtain 15 mg (99.6%) of the desired product as an orange powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07612070B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-9a524bbb59154315ac3ea19863162007 |
| Source note | uspto-grants-2009_11 |