反应详情

温度

0 °C

Dissolve 3,4,5-trimethoxybenzoyl chloride (2.3 g, 10 mmol) and N,O-dimethylhydroxylamine hydrochloride (1.10 g, 11 mmol) in ethanol-free chloroform at room temperature. Cool the solution to 0° C. and add pyridine (1.85 g, 22 mmol). Stir at ambient temperature for 1 hour and evaporate the solvent in vacuo. Partition the residue between aqueous sodium chloride and a 1:1 mixture of ethyl ether and methylene chloride. Separate the organic phase, dry (Na2SO4), and evaporate the solvent in vacuo to yield an oil. Filter the oil through silica gel eluting with 65% ethyl acetate/hexane to yield 2.5 g of N-methoxy-N-methyl-(3,4,5-trimethoxy)benzamide.

1. customevaporate the solvent in vacuo
2. customPartition the residue between aqueous sodium chloride
3. additiona 1:1 mixture of ethyl ether and methylene chloride
4. customSeparate the organic phase
5. dry with materialdry (Na2SO4)
6. customevaporate the solvent in vacuo
7. customto yield an oil
8. filtrationFilter the oil through silica gel eluting with 65% ethyl acetate/hexane