Triethylamine → 2-Amino-5-nitro-N-(5-phenoxy-thiophen-2-ylmethyl)-nicotinamide

Then, the resulting lithium salt of 2-amino-5-nitro-nicotinic acid, C-(5-phenoxy-thiophen-2-yl)-methylamine (60 mg, 0.29 mmol), benzotriazol-1-yl-tris(dimethylamino)phosphonium hexafluorophosphate (162 mg, 0.367 mmol) and triethylamine (103 μl, 0.735 mmol) were dissolved in N,N-dimethylformamide (2.0 mL), and the solution was stirred for 6 hours at room temperature. Water was added to the reaction solution, which was then extracted with ethyl acetate, and the organic layer was washed with water and brine. The solvent was evaporated in vacuo, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1), and the title compound (87 mg, 0.24 mmol, 96%) was obtained as a pale yellow solid.

1. extractionwas then extracted with ethyl acetate
2. washthe organic layer was washed with water and brine
3. customThe solvent was evaporated in vacuo
4. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)

ORDレコード

ord-318f5f89d8034bb6af286aee58aeef8e

出典データセット

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07932272B2