Tetrahydrofuran → HCID 21201685, 화합물

1-[1-(2-Toluoylmethy)-2-oxo-5-(2-pyridylcarbonyl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(3-ethoxycarbonylphenyl)urea (466 mg) was dissolved in methanol (22 ml), aqueous lithium hydroxide monohydrate (158 mg) solution (11 mg) and tetrahydrofuran (11 ml) were added, and the mixture was refluxed for one hour. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in water, the solution was washed with diethyl ether, acidified with 1N hydrochloric acid, and extracted with methylene chloride. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Isopropyl ether was added to the residue for trituration, collected by filtration, to thereby obtain 203 mg of the titled compound.

1. temperaturethe mixture was refluxed for one hour
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. dissolutionthe residue was dissolved in water
4. washthe solution was washed with diethyl ether
5. extractionextracted with methylene chloride
6. washThe organic layer was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was evaporated under reduced pressure
9. additionIsopropyl ether was added to the residue for trituration
10. filtrationcollected by filtration

ORD 기록

ord-9233b9f48e4d4212a51aedc569fc805d

출처 데이터셋

uspto-grants-2001_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06239131B1