Water → 3-[[2'-(1-Triphenylmethyltetrazol-5-yl)biphenyl-4-yl]methyloxy]-4-nitrobenzoic acid morpholide

The compound ([3]-(32)-587) (0.99 g) prepared in Example 36 was dissolved in dry N,N-dimethylformamide (19 ml), and 50% sodium hydride (0.20 g) was added to the solution. The mixture was stirred at room temperature for 15 minutes. A solution of N-(triphenylmethyl)-5-[4'-(bromomethyl)biphenyl-2-yl]tetrazole (2.19 g) in N,N-dimethylformamide (6.5 ml) was added to the solution. The mixture was stirred at room temperature for 39 hours. The reaction mixture was added to water (50 ml), and extracted with chloroform (100 ml). The organic layer was washed, dried over anhydrous sodium sulfate, and concentrated to obtain the compound (2.72 g) as a light yellow solid. The product was purified by silica gel column chromatography (Kieselgel 60=190 g, chloroform/ethyl acetate=7/3) to obtain the compound ([3]-(33)-587) (1.41 g).

1. stirringThe mixture was stirred at room temperature for 39 hours
2. extractionextracted with chloroform (100 ml)
3. washThe organic layer was washed
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated

ORDレコード

ord-0ad033c75743437fa014d79e0580e8dc

出典データセット

uspto-grants-1998_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05739131