HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-Iodosuccinimide → HCID 22050117, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-Iodosuccinimide | HCID 120273 | — |
| Reactant | 4-benzyloxy-1-(3-fluorobenzyl)-1H-pyridin-2-one | HCID 22050222 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 22050117 | HCID 22050117 | 90.6% |
Reaction Steps
Heated a reaction mixture of 4-(benzyloxy)-1-(3-fluorobenzyl)pyridin-2(1H)-one (4.83 g, 15.6 mmol) in anhydrous acetonitrile (55 mL) and N-iodosuccinimide (NIS, 3.86 g, 17.1 mmol) under nitrogen atmosphere at 650 C for 4 h. The reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography (silica gel) using EtOAc/hexanes (1:1 v:v). The appropriate fractions were collected according to ES MS (M+H 436) and washed with Na2SO3 to remove the color impurities. The fractions were concentrated under reduced pressure and dried in vacuo to afford the desired product (6.15 g, 90%) as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07067540B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-ec539c599c0d411f8ec888a3ccce30f8 |
| Source note | uspto-grants-2006_06 |