HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Phenylbutyric Acid → Methyl 3-methoxy-4-[6-(2-phenylbutanamido)benzimidazol-1-ylmethyl]benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Phenylbutyric Acid | HCID 7012 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | Methyl 4-(6-aminobenzimidazol-1-ylmethyl)-3-methoxybenzoate | HCID 14763098 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 3-methoxy-4-[6-(2-phenylbutanamido)benzimidazol-1-ylmethyl]benzoate | HCID 23365891 | 25% |
Reaction Steps
A solution of 1,1'-carbonyldiimidazole (0.23 g.) and 2-phenylbutyric acid (0.22 g.) in dichloromethane (3 ml.) was heated under reflux for 30 minutes and then treated with a solution of (J) (0.41 g.) in dichloromethane (3 ml.). The mixture was heated under reflux for an additional 10 minutes and then diluted with dichloromethane. This mixture was washed successively with 10% v/v hydrochloric acid, water, and brine, then dried (MgSO4) and evaporated. The resultant residue was purified by flash chromatography on a 5×25 cm. silica gel column using 3:97 v/v methanol:dichloromethane as the eluent to give the title compound (0.15 g., 25%): partial NMR: 2.0(br m,2H, CH3CH2), 3.4(t,1H, CH2CH), 7.3(s,5H, Ar).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04859692 |
| Source dataset | uspto-grants-1989_08 |
| ORD ID | ord-ab0af418cc8f411a9072a4e33e9c1ef6 |
| Source note | uspto-grants-1989_08 |