HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethyl orthoformate → 1H-Benzimidazole-5-carboxylic acid, 7-iodo-, methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | Methyl 3,4-diamino-5-iodobenzoate | HCID 67512100 | — |
| Catalyst | p-Toluenesulfonic acid | HCID 6101 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1H-Benzimidazole-5-carboxylic acid, 7-iodo-, methyl ester | HCID 59627771 | 45.1% |
Reaction Steps
To a solution of 3,4-diamino-5-iodo-benzoic acid methyl ester (1.68 g, 5.75 mmol) in THF (20 mL) was added trimethyl orthoformate (1.26 mL, 11.5 mmol) and 4-toluenesulfonic acid (11 mg, 0.057 mmol). The mixture was stirred at room temperature overnight, then partitioned between ethyl acetate and water. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to give 783 mg (45%) of 7-Iodo-3H-benzoimidazole-5-carboxylic acid methyl ester, MS (M+H)=303.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476457B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-1266960ff17c4bc599b574c5960c6c30 |
| Source note | uspto-grants-2013_07 |