HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21201854, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2-Ethylbutyryl chloride | HCID 75954 | — |
| 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 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 21201854 | HCID 21201854 | 111.9% |
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-ethyl-n-butanoyl chloride (144 mg) and pyridine (87 μl) were added thereto, the mixture was refluxed for 2 hours. Water (100 ml) and ethyl acetate (100 ml) were added to the reaction mixture, and separated. The organic layer was washed with 1N hydrochloric acid, 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 666 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-34f834d068ff4641922538ee4c798d4c |
| Source note | uspto-grants-2001_05 |