تفاعل #95403

معادلة التفاعل

hydrochloric acid

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

methanol

methanol

→

aimed compound

المردود 52.1%

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

المردود 52.1%

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر