HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon Dioxide → HCID 69134282, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon Dioxide | HCID 280 | — |
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 69135170 | HCID 69135170 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Product | HCID 69134282 | HCID 69134282 | 91% |
Reaction Steps
10 g (29 mmol) 4-Benzyloxy-6-bromo-2-ethyl-1-methyl-1H-benzimidazole, 4.6 g (17.4 mmol) triphenylphosphine, 1.0 g (4.3 mmol) palladium(II) acetate in 145 ml (290 mmol) dimethylamine (2 M in THF) were transferred to an autoclave and carbonylated (6 bar CO2) at 120° C. for 24 h. The catalyst was filtered off and the filtrate was concentrated in vacuo. Purification of the residue by column chromatography on silica gel (dichloromethane/methanol=93:7) and crystallization from diethyl ether afforded 11.3 g (91%) of the title compound as white crystals. m.p. 104°-108° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07307084B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-6b75b37eed8c459b943f4213e12977b9 |
| Source note | uspto-grants-2007_12 |