반응 #95403

반응 방정식

hydrochloric acid

3-(9-methoxy-3-hydroxy-5,9-dimethyl-decanoyl)-4-butyrolactone

methanol

methanol

→

aimed compound

수율 52.1%

3-[1,9-dimethoxy-5,9-dimethyl-2(E)decenylidene]-4-butyrolactone

수율 52.1%

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe solvent is distilled off in vacuo
2. 2
   workup.DISSOLUTIONthe residue is dissolved in ether
3. 3
   세척the etheral solution is washed with distilled water
4. 4
   기타dried
5. 5
   workup.DISTILLATIONthe solvent is distilled off
6. 6
   기타the residue is purified by column chromatography (adsorbent
7. 7
   workup.ADDITIONKieselgel 60, solvent: a 10:0.1 mixture of benzene and methanol)

실험 절차

1 ml of methanol saturated with hydrochloric acid is added to a solution of 1.05 g (0.0033 moles) of 3-(9-methoxy-3-hydroxy-5,9-dimethyl-decanoyl)-4-butyrolactone in 10 ml of dry methanol, and the mixture is allowed to stand at room temperature overnight. The solvent is distilled off in vacuo, the residue is dissolved in ether, the etheral solution is washed with distilled water, dried, the solvent is distilled off, and the residue is purified by column chromatography (adsorbent: Kieselgel 60, solvent: a 10:0.1 mixture of benzene and methanol). 0.54 g (52.1%) of the aimed compound are obtained; Rf =0.8 (developed with a 10:0.2 mixture of benzene and methanol).

출처