1,10-Phenanthroline → 3-Benzooxazol-2-yl-azetidine-1-carboxylic acid benzyl ester

온도

90 °C

To 195 mg (0.45 mmol) 3-(2-iodo-phenylcarbamoyl)-azetidine-1-carboxylic acid benzyl ester in 4.5 mL DME in a sealed tube under nitrogen were added 291 mg (0.89 mmol) Cs2CO3, 8.1 mg (44.6 μmol) 1,10-phenanthroline, 4.3 mg (22.3 μmol) CuI, and the mixture was heated at 90° C. for 16 hours. After cooling to room temperature, 5 mL H2O was added followed by 4 drops 1 M HCl, 5 mL NaHCO3 and the mixture was extracted with DCM (3×10 mL). The organic layers were combined and dried with Na2SO4. After filtration and evaporation of the solvent the product was purified by preparative HPLC.

1. temperatureAfter cooling to room temperature
2. extractionthe mixture was extracted with DCM (3×10 mL)
3. dry with materialdried with Na2SO4
4. filtrationAfter filtration and evaporation of the solvent the product
5. customwas purified by preparative HPLC

ORD 기록

ord-5cd5c7b326da43ec8c639dd15612c781

출처 데이터셋

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09346816B2