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

HRID 67125
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인쇄 미리보기

반응식

HRID 67125 반응식
Cl.[CH3:2][O:3][C:4]([CH3:23])([CH3:22])[CH2:5][CH2:6][CH2:7][CH:8]([CH3:21])[CH2:9][CH:10](O)[CH2:11][C:12]([CH:14]1[CH2:19][O:18][C:16](=[O:17])[CH2:15]1)=[O:13].[CH3:24]O>>[CH3:24][O:13][C:12](=[C:14]1[CH2:19][O:18][C:16](=[O:17])[CH2:15]1)/[CH:11]=[CH:10]/[CH2:9][CH:8]([CH3:21])[CH2:7][CH2:6][CH2:5][C:4]([O:3][CH3:2])([CH3:23])[CH3:22]
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참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887Methanol2회HCID 20528523HCID 20528523, 화합물

생성물 1

HCID 867385323-[1,9-dimethoxy-5,9-dimethyl-2(E)decenylidene]-4-butyrolactone수율 52.1%

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).

후처리

  1. distillationThe solvent is distilled off in vacuo
  2. dissolutionthe residue is dissolved in ether
  3. washthe etheral solution is washed with distilled water
  4. customdried
  5. distillationthe solvent is distilled off
  6. customthe residue is purified by column chromatography (adsorbent
  7. additionKieselgel 60, solvent: a 10:0.1 mixture of benzene and methanol)

출처 및 근거

ORD 기록
ord-71a010aa3742498d8fbca5124bc9b087
출처 데이터셋
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04344959

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