反応 #41790

反応方程式

4-(4-methylamino-3-nitro-phenoxy)-pyridine-2-carboxylic acid

EDC-HCl

HOAT

diisopropylethylamine

2,2-dimethyl-oxazolidine

→

4-(4-Methylamino-3-nitro-phenoxy)-pyridine-2-carboxylic acid (2-hydroxy-ethyl)-amide

溶媒

ethyl acetate

THF

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   workup.ADDITIONwas added
3. 3
   洗浄washed with water
4. 4
   洗浄The aqueous layer was washed with ethyl acetate
5. 5
   乾燥dried over MgSO4
6. 6
   ろ過filtered
7. 7
   濃縮concentrated

実験手順

To a suspension of the 4-(4-methylamino-3-nitro-phenoxy)-pyridine-2-carboxylic acid (1 eq) in dry THF, EDC-HCl (1.2 eq), HOAT (1.2 eq), and diisopropylethylamine (3 eq) were added. The suspension was stirred for 10 minutes whereupon 2,2-dimethyl-oxazolidine (1.1 eq) was added and the solution is allowed to stir overnight. The mixture was then diluted with ethyl acetate and washed with water. The aqueous layer was washed with ethyl acetate, the organic layers combined, dried over MgSO4, filtered, and concentrated. LCMS m/z 333.2 (MH+), tR=2.1 min.

出典