HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 69135061, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 69135079 | HCID 69135079 | — |
| Product | HCID 69135061 | HCID 69135061 | 64% |
Reaction Steps
A suspension of 3.8 g (10.7 mmol) (6-bromo-1,2-dimethyl-1H-benzimidazol-4-yl)-(1-phenyl-allyl)-amine and 3.5 g p-toluenesulphonic acid monohydrate in 80 ml toluene was refluxed for 26 h. The suspension was poured into a mixture of 50 ml saturated sodium hydrogencarbonate solution and 150 ml water and extracted with ethyl acetate. The organic phase was separated, dried over anhydrous magnesium sulfphate and evaporated. The residue was purified by column chromatography on silica gel (toluene/dioxane/methanol=6:3.8:0.2). Crystallization from diisopropyl ether gave 2.45 g (64%) of the title compound as a colourless solid. m.p. 186-189° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07307084B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-ddd0835610034fe9853a1159313a18d1 |
| Source note | uspto-grants-2007_12 |