HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromobenzene → HCID 11260802, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromobenzene | HCID 7961 | — |
| Reactant | HCID 22052381 | HCID 22052381 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 11260802 | HCID 11260802 | — |
Reaction Steps
A mixture of 100 mg (0.2 mmol) 3-[2-(2,4-Dichloro-phenyl)-ethoxy]-4-methoxy-N-piperidin-4-ylmethyl-benzamide, 50 mg (0.32 mmol) Bromobenzene, 70 mg sodium-t-butoxide in 5 ml dioxane were purged with argon for 10 min. Then 37 mg of 2-(Dicyclohexylphosphino)biphenyl and 20 mg Pd2(dba)3 were added under argon and the mixture refluxed overnight. The residue was taken up in 3 ml saturated NaHCO3 solution and filtered through a chem elut® cartridge by elution with ethyl acetate. Subsequent removal of the solvent under reduced pressure and purification by preparative HPLC (C18 reverse phase column, elution with a H2O/MeCN gradient with 0.5% TFA) the fractions containing the product were evaporated and lyophilised.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06953857B2 |
| Source dataset | uspto-grants-2005_10 |
| ORD ID | ord-2b38b0bd3b4d4ccf9a8bb72067a089cc |
| Source note | uspto-grants-2005_10 |