반응 #443822

반응 방정식

ammonium chloride

2-(5-acetylamino-2-methoxyphenyl)-1,3-dioxolane

NaH

methyl iodide

→

2-[5-(N-acetyl-N-methylamino)-2-methoxyphenyl]-1,3-dioxolane

수율 94.3%

용매

DMF

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGstirred at room temperature for 1 hr
2. 2
   기타And to the resulted reaction mixture
3. 3
   추출extracted with CH2Cl2
4. 4
   세척The extract was washed with water and brine
5. 5
   건조dried over Na2SO4
6. 6
   농축concentrated in vacuo

실험 절차

A solution of 2-(5-acetylamino-2-methoxyphenyl)-1,3-dioxolane (5.0 g, 21.1 mmol) in DMF (16 ml) was added to a suspension of NaH (1.0 g, 25.3 mmol) in DMF (5 ml) and then the mixture was stirred at room temperature for 10 min. To the mixture was added methyl iodide (3.6 g, 25.3 mmol) and then stirred at room temperature for 1 hr. And to the resulted reaction mixture was added ammonium chloride and then extracted with CH2Cl2. The extract was washed with water and brine, dried over Na2SO4 and concentrated in vacuo to give crude 2-[5-(N-acetyl-N-methylamino)-2-methoxyphenyl]-1,3-dioxolane (5.0 g, 94%) as a orange oil.

출처