HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylamine → HCID 86588556, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | Methyl 3-fluoro-4-nitrobenzoate | HCID 592761 | — |
| Reactant | (1H-benzo[d]imidazol-2-yl)methanamine dihydrochloride | HCID 2723957 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 86588556 | HCID 86588556 | 85% |
Reaction Steps
To a flask under nitrogen atmosphere was charged 500 ml of NMP and 3-fluoro-4 nitro benzoic acid methylester (15.64 g, 78.5 mmol, 1 eq) followed by aminomethyl-benzimidazole dihydrochloride (20.16 g, 91.6 mmol, 1.2 eq). To this, Diispropyl ethylamine (55 ml, 316 mmol, 4 eq) was charged and stirred for 16 hours. The reaction was then poured into 1200 ml of ice water resulting in a yellow/orange solid. The solid was filtered and resuspended in 300 ml of cold water, stirred for 1 hour, filtered and dried to constant weight. Yield 85%, 18.8 g. TLC elution solvent system 5% methanol/95% dichloromethane, Rf=0.6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07030150B2 |
| Source dataset | uspto-grants-2006_04 |
| ORD ID | ord-1c818322919a4ad8a46368921bee7eac |
| Source note | uspto-grants-2006_04 |