Nitrogen → HCID 67365317、化合物

温度

0 °C

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 5-(3-chloro-phenyl)-2-methyl-oxazole-4-carboxylic acid (2-{2-[1-(tert-butyl-dimethyl-silanyloxy)-ethyl]-oxazol-5-ylmethyl}-2H-[1,2,3]triazol-4-yl)-amide (106 mg, 0.20 mmol) in dry THF (1.9 mL) was treated at 0° C. with TBAF (0.39 mL of a 1M solution in THF, 0.39 mmol). The reaction mixture was stirred at 0° C. for 45 min. The mixture was then diluted with EA (10 mL), washed with NaHCO3 (10 mL) followed by brine (3×10 mL), dried over MgSO4, filtered and concentrated under reduced pressure. Purification of the residue by FC (19:1 CH2Cl2-MeOH) gave the title compound as a white solide. TLC:rf (19:1 CH2Cl2-MeOH)=0.22. LC-MS-conditions 01: tR=0.93 min; [M+H]+=428.97.

1. washwashed with NaHCO3 (10 mL)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customPurification of the residue by FC (19:1 CH2Cl2-MeOH)

ORDレコード

ord-89c6c46c2a094939a7dad70d1bd049ed

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08536209B2