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Pyridine → 2,6,6-Trimethyl-1-(3-acetoxy-but-1-ynyl)cyclohexa-1,3-diene

HRID 1156627
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1156627
[CH3:1][C:2]1[C:3](O)([C:10]#[C:11][CH:12]([OH:14])[CH3:13])[C:4]([CH3:9])([CH3:8])[CH2:5][CH2:6][CH:7]=1.N1C=CC=CC=1.[C:22](OC(=O)C)(=[O:24])[CH3:23]>C(OC)(C)(C)C>[CH3:1][C:2]1[CH:7]=[CH:6][CH2:5][C:4]([CH3:9])([CH3:8])[C:3]=1[C:10]#[C:11][CH:12]([O:14][C:22](=[O:24])[CH3:23])[CH3:13]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 140863082,6,6-Trimethyl-1-hydroxy-1-(3-hydroxy-but-1-ynyl)cyclohex-2-ene

Produkt 1

HCID 155179992,6,6-Trimethyl-1-(3-acetoxy-but-1-ynyl)cyclohexa-1,3-dieneAusbeute 45 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 15413tert-Butyl methyl etherLösungsmittel

Versuchsvorschrift

In a 500 ml. three-necked flask fitted with a mechanical stirrer, a dropping funnel, a thermometer and a reflux condenser protected by a calcium chloride tube is placed a mixture of 66 g. of 2,6,6-trimethyl-1-hydroxy-1-(3-hydroxy-but-1-ynyl)cyclohex-2-ene and 76 g. of pyridine in 200 ml. of tertiary butylmethyl ether. To the stirred solution is added 34 g. of acetic anhydride at room temperature. The reaction mixture is stirred for a period of 27 hours at ambient temperature. The reaction mixture is then poured into 200 ml. of water and the organic layer is separated, washed with 10% hydrochloric acid, subsequently with water, 10% sodium bicarbonate solution and water, and finally dried over sodium sulfate. Concentration yields a residue which gives on distillation 33 g. or 45% yield of 2,6,6-trimethyl-1-(3-acetoxy-but-1-ynyl)cyclohexa-1,3-diene, b.p. 125° C./1 mm., nD20 1.5045.

Aufarbeitung

  1. customthree-necked flask fitted with a mechanical stirrer, a dropping funnel
  2. customa thermometer and a reflux condenser protected by a calcium chloride tube
  3. additiona mixture of 66 g
  4. additionTo the stirred solution is added 34 g
  5. customat room temperature
  6. additionThe reaction mixture is then poured into 200 ml
  7. customof water and the organic layer is separated
  8. washwashed with 10% hydrochloric acid, subsequently with water, 10% sodium bicarbonate solution and water
  9. dry with materialfinally dried over sodium sulfate
  10. concentrationConcentration
  11. customyields a residue which
  12. customgives on distillation 33 g

Quellen und Nachweise

ORD-Eintrag
ord-a84a909cdd25434c98370702d396613b
Quelldatensatz
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04336401

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