HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 5-Dibenzylamino-6-fluoro-N-methyl-N-propyl-isophthalamic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | N-Methylpropylamine | HCID 12315 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Reactant | 5-Dibenzylamino-4-fluoro-isophthalic acid 3-ethyl ester | HCID 68814612 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-Dibenzylamino-6-fluoro-N-methyl-N-propyl-isophthalamic acid ethyl ester | HCID 68814435 | 65% |
Reaction Steps
Dissolve the 1-hydroxybenzotriazole hydrate (139 mg, 1.03 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (197 mg, 1.03 mmol) and 5-dibenzylamino-4-fluoro-isophthalic acid 3-ethyl ester (381 mg, 0.934 mmol) in dichloromethane (10.0 mL). Stir for 30 min. Add methylpropyl amine (68.3 mg, 0.93 mmol) to the reaction mixture. Stir the reaction for 4 h. Add 10% aqueous potassium carbonate solution (10 mL). Extract with dichloromethane (2×50 mL). Combine the organic layers, wash with water (20 mL), saturated aqueous sodium chloride (20 mL), dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 40:60 ethyl acetate:hexanes) to give the title compound (279 mg, 65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07585885B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-eaee806a0c2041d7b74918d01ce8daf2 |
| Source note | uspto-grants-2009_09 |