HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 21201595, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2-Propylvaleryl chloride | HCID 76240 | — |
| Reactant | 1-[1-(2-toluoylmethyl)-2-oxo-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(3-ethoxycarbonylphenyl)urea | HCID 21201630 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 21201595 | HCID 21201595 | 100.4% |
Reaction Steps
1-[1-(2-Toluoylmethyl)-2-oxo-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(3-ethoxycarbonylphenyl)urea(500 mg) obtained from Step 1 of Example 93 was suspended in 1,2-dichloroethane (10 ml), 2-n-propylpentanoyl chloride (174 mg) and pyridine (87 μl) were added, the mixture was refluxed for 2 hours. The reaction mixture was allowed to cool, successively washed with 1N hydrochloric acid and saturated aqueous sodium bicarbonate, dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography(n-hexane:ethyl acetate=2:1), to thereby obtain 625 mg of the titled compound (Yield: 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06239131B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-30b426013d1a4ca387e610f616c77cf4 |
| Source note | uspto-grants-2001_05 |