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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1979381Generated: October 30, 2026

Water → HCID 21201854, compound

https://huagongshe.com/reaction/1979381

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantPyridineHCID 1049—
Reactant2-Ethylbutyryl chlorideHCID 75954—
Reactant1-[1-(2-toluoylmethyl)-2-oxo-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(3-ethoxycarbonylphenyl)ureaHCID 21201630—
Solvent1,2-DichloroethaneHCID 11—
SolventEthyl AcetateHCID 8857—
ProductHCID 21201854HCID 21201854111.9%

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

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06239131B1
Source datasetuspto-grants-2001_05
ORD IDord-34f834d068ff4641922538ee4c798d4c
Source noteuspto-grants-2001_05