HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dibenzylamine → HCID 178420338, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dibenzylamine | HCID 7656 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 6-Bromo-1H-benzimidazole | HCID 785299 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | 2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl | HCID 2734217 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Product | HCID 178420338 | HCID 178420338 | — |
Reaction Steps
The compound was synthesized starting from 5-bromobenzimidazole (200 mg; 1 mmol; 1 eq.), dibenzylamine (0.231 ml; 1.2 mmol; 1.2 eq.), 2-dicyclohexylphosphino-2′-(N,N-dimethylamino)biphenyl (9 mg; 0.024 mmol; 0.024 eq.; 2.4 mol %), Pd2 dba3 (9 mg; 0.01 mmol; 0.01 eq.; 1 mol %) and lithiumbis(trimethylsilyl)amide 1 M in THF (2.2 ml; 2.2 mmol; 2.2 eq.) according to method 1 but purified by flash chromatography on silica using a CHCl3/MeOH gradient; Yield: 0.127 g (41%); 314.1 MS m/z: [M+H]+; 1H-NMR (500 MHz, DMSO d6): δ 4.67 (s, 4H); 6.70 (br s, 1H); 6.73 (dd, 1H, 4J=2.4 Hz, 3J=8.9 Hz); 7.19-7.23 (m, 2H); 7.28-7.33 (m, 9H); 7.90 (s, 1H); 11.91 (br s, 1H); HPLC (METHOD [A]): rt 14.79 min (99.2%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08541596B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-3c812b5ab0ba448a972a6a1f6eddbd55 |
| Source note | uspto-grants-2013_09 |