HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethylsilyl cyanide → (8-methoxy-4H-benzo[1,3]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | 8-methoxy-4H-benzo[1,3]dioxine-6-carbaldehyde | HCID 13266818 | — |
| Reactant | 4-(5-Methyl-1,2,4-oxadiazol-3-yl)aniline | HCID 18188176 | — |
| Catalyst | Ytterbium triflate | HCID 2733225 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (8-methoxy-4H-benzo[1,3]dioxin-6-yl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile | HCID 59517220 | — |
Reaction Steps
To a solution of 3.5 g of Yb(OTf)3 in 250 ml of THF there were added 9.8 g of 4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamine, 10.8 g of 8-methoxy-4H-benzo[1,3]dioxine-6-carbaldehyde, 10 g of MS3A and 15 ml of trimethylsilyl cyanide under a nitrogen atmosphere, and the mixture was stirred overnight at room temperature. The reaction mixture was filtered through celite, and the celite was washed with 1000 ml of ethyl acetate. The organic layer was concentrated under reduced pressure to give the title compound (29.2 g, crude product) as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163787B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-83a0d23a3b8c44d9ade7a84a7cf462bb |
| Source note | uspto-grants-2012_04 |