反応 #1869212

反応方程式

ethyl acetate

(2,4-dimethoxyphenyl)acetic acid

N,N-carbonyldiimidazole

methyl amine

→

subtitled compound

収率 73.3%

2-(2,4-Dimethoxyphenyl)-N-methylacetamide

収率 73.3%

溶媒

DMF

H2O

反応条件

後処理

1. 1
   workup.STIRRINGthe reaction mixture was stirred at room temperature over the week-end
2. 2
   乾燥The organic layer was dried over Na2SO4
3. 3
   ろ過filtered
4. 4
   濃縮concentrated
5. 5
   その他The residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit)

実験手順

A mixture of (2,4-dimethoxyphenyl)acetic acid (577 mg, 3.0 mmol) and N,N-carbonyldiimidazole (608 mg, 3.75 mmol) in DMF (10 mL) was stirred at room temperature for 45 min, aqueous 40% methyl amine (4.5 mL) was added and the reaction mixture was stirred at room temperature over the week-end. The reaction mixture was is partitoned between ethyl acetate and H2O. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel flash chromatography (0-80% ethyl acetate in petroleum spirit) to give the subtitled compound (460 mg).

出典