Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- → HCID 20164219, Verbindung

HRID 66465

Reaktionsgleichung

Reaktionsgleichung von HRID 66465
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][N+:13]([O-:15])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].I[CH2:17][CH2:18][C:19](=[O:28])[CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([N+:13]([O-:15])=[O:14])[CH2:17][CH2:18][C:19](=[O:28])[CH2:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Komponenten

4

Edukt 2

HCID 10036050Benzene, 1,2-dimethoxy-4-(2-nitroethyl)-HCID 20164202HCID 20164202, Verbindung

Produkt 1

HCID 20164219HCID 20164219, VerbindungAusbeute 113,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of 36 g (0.17 mole) of 2-(3,4-dimethoxyphenyl)-1-nitroethane in 300 mL of dry tetrahydrofuran was added 71 g (0.17 mole) of 40% Triton B. The solution was stirred at room temperature for 10 min. 55.3 g (0.19 mole) of 1-iodo-5-phenyl-3-pentanone in a minimum amount of dry tetrahydrofuran was added dropwise. The mixture was stirred at room temperature for 30 min, at 50° C. for 3 hr., then allowed to stir at room temperature overnight. Solvent was removed in vacuo and the residue taken up in ether and extracted twice with water. The organic layer was dried over anh Mg SO4, and concentrated at reduced pressure to give 71.5 g of crude oil. This crude material was passed through HPLC to give 46.4 g. of purified material.

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for 30 min, at 50° C. for 3 hr
  2. stirringto stir at room temperature overnight
  3. customSolvent was removed in vacuo
  4. extractionextracted twice with water
  5. dry with materialThe organic layer was dried over anh Mg SO4
  6. concentrationconcentrated at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c067a0383e4d4285a429c03fc770b411
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04342692

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