반응 #1051981

반응 방정식

Pyrrolidine

2-bromomethyl-5-formylamino-2,4,6,7-tetramethyl-2,3-dihydrobenzofuran

→

desired compound

수율 83.5%

5-Amino-2,4,6,7-tetramethyl-2-pyrrolidinomethyl-2,3-dihydrobenzofuran

수율 83.5%

용매

water

반응 조건

후처리

1. 1
   온도After the reaction mixture was cooled
2. 2
   추출the product was extracted with ethylacetate
3. 3
   세척The extract was washed with water
4. 4
   기타dried
5. 5
   workup.DISTILLATIONthe solvent was distilled off
6. 6
   기타The residue was purified by column chromatography on silica gel (chloroform-methanol, 9:1)
7. 7
   기타recrystallized from hexane

실험 절차

Pyrrolidine (20 ml) was added to 2-bromomethyl-5-formylamino-2,4,6,7-tetramethyl-2,3-dihydrobenzofuran (3.0 g, 9.6 mmol) and the mixture was heated at 160° C. in an autoclave for 15 hours. After the reaction mixture was cooled, the mixture was diluted with water and the product was extracted with ethylacetate. The extract was washed with water and dried and then the solvent was distilled off. The residue was purified by column chromatography on silica gel (chloroform-methanol, 9:1) and recrystallized from hexane to obtain the desired compound (2.2 g, yield: 83.5%), m.p. 85°-86° C. (dec.).

출처