HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22504408, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Fluorobenzyl bromide | HCID 68021 | — |
| Reactant | HCID 22504439 | HCID 22504439 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22504408 | HCID 22504408 | — |
Reaction Steps
To a solution of the compound obtained in Example 31 (1) (0.4 kg) in N,N-dimethylformamide (160 ml), 60% sodium hydride (0.065 g) was added at 0° C. under nitrogen atmosphere and the mixture was stirred for 20 minutes, followed by addition of 4-fluorobenzyl bromide (0.2 ml), and the mixture was stirred at 15 to 30° C. for 15 hours. The reaction solution was then poured into water and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was separated using silica gel column chromatography (hexane:ethyl acetate=1:3) to obtain 0.3882 g of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07612070B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-05942842c4fc48fe85013018369c7e1c |
| Source note | uspto-grants-2009_11 |