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Methyl iodide → 1,4-Dimethoxy-2,5-bis(methoxymethoxy)-3-methyl-6-{5-[2,5-dimethoxy-3,6-bis(methoxymethoxy)phenyl]pentyl}benzene

HRID 1588149
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1588149
[CH3:1][O:2][C:3]1[C:8]([O:9][CH2:10][O:11][CH3:12])=[CH:7][C:6]([O:13][CH3:14])=[C:5]([O:15][CH2:16][O:17][CH3:18])[C:4]=1[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][C:24]1[C:29]([O:30][CH2:31][O:32][CH3:33])=[C:28]([O:34][CH3:35])[CH:27]=[C:26]([O:36][CH2:37][O:38][CH3:39])[C:25]=1[O:40][CH3:41].[CH3:42]N(C)P(=O)(N(C)C)N(C)C.C([Li])(CC)C.CI>O1CCCC1.C(OCC)C.C1C=CC=CC=1>[CH3:1][O:2][C:3]1[C:4]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][C:24]2[C:29]([O:30][CH2:31][O:32][CH3:33])=[C:28]([O:34][CH3:35])[CH:27]=[C:26]([O:36][CH2:37][O:38][CH3:39])[C:25]=2[O:40][CH3:41])=[C:5]([O:15][CH2:16][O:17][CH3:18])[C:6]([O:13][CH3:14])=[C:7]([CH3:42])[C:8]=1[O:9][CH2:10][O:11][CH3:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 6328Methyl iodideHCID 12679HexamethylphosphoramideHCID 136460702,2'-Pentamethylene-bis[1,4-dimethoxy-3,6-bis(methoxymethoxy)benzene]HCID 178418400CID 53628100

Produkt 1

HCID 136460751,4-Dimethoxy-2,5-bis(methoxymethoxy)-3-methyl-6-{5-[2,5-dimethoxy-3,6-bis(methoxymethoxy)phenyl]pentyl}benzene

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 8028TetrahydrofuranLösungsmittelHCID 22174802Benzene etherLösungsmittel

Versuchsvorschrift

140 Milligrams of 2,2'-pentamethylene-bis[1,4-dimethoxy-3,6-bis(methoxymethoxy)benzene] was dissolved in 5 ml of anhydrous tetrahydrofuran under argon gas stream conditions, then 0.5 ml of hexamethylphosphoric triamide was added to this solution and the mixture was cooled in a dry ice-acetone bath. Next, 0.23 ml of sec-butyllithium (1.4M, cyclohexane solution) was added dropwise to the reaction mixture and stirred for 1 hour. Then, 0.06 ml of methyl iodide was added dropwise thereto under cooling in a dry ice-acetone bath for 12 hours with stirring. The solvent was removed by evaporation under reduced pressure, to the residue obtained was added 100 ml of a mixed solvent of diethyl ether-benzene (1:1), and the organic layer was washed with water then with a saturated sodium chloride aqueous solution, and dried over anhydrous magnesium sulfate. The dried solution was concentrated under reduced pressure to obtain 100 mg of 1,4-dimethoxy-2,5-bis(methoxymethoxy)-3-methyl-6-{5-[2,5-dimethoxy-3,6-bis(methoxymethoxy)phenyl]pentyl}benzene. Colorless needles crystals.

Aufarbeitung

  1. temperaturethe mixture was cooled in a dry ice-acetone bath
  2. temperatureunder cooling in a dry ice-acetone bath for 12 hours
  3. stirringwith stirring
  4. customThe solvent was removed by evaporation under reduced pressure, to the residue
  5. customobtained
  6. washthe organic layer was washed with water
  7. dry with materialwith a saturated sodium chloride aqueous solution, and dried over anhydrous magnesium sulfate
  8. concentrationThe dried solution was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d1b618cb66e1473c8eb668000644d0a5
Quelldatensatz
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05220042

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