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1,2-Dichloroethane → HCID 11678369, Verbindung

HRID 1296588
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1296588
[CH2:1]([C:8]1[NH:16][C:15]2[C:14](=[O:17])[N:13]([CH2:18][CH2:19][CH3:20])[C:12](=[O:21])[N:11]([CH2:22][CH2:23][C:24]3[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][CH:25]=3)[C:10]=2[N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[CH2:39]([NH:41][CH2:42][CH2:43][OH:44])[CH3:40].Cl[CH2:46][CH2:47]Cl>>[CH2:1]([C:8]1[N:16]([CH2:40][CH2:39][N:41]([CH2:46][CH3:47])[CH2:42][CH2:43][OH:44])[C:15]2[C:14](=[O:17])[N:13]([CH2:18][CH2:19][CH3:20])[C:12](=[O:21])[N:11]([CH2:22][CH2:23][C:24]3[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][CH:25]=3)[C:10]=2[N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 111,2-DichloroethaneHCID 80722-(Ethylamino)ethanolHCID 10340Sodium CarbonateHCID 103655718-Benzyl-3-[2-(4-nitrophenyl)ethyl]-1-propylxanthine

Produkt 1

HCID 11678369HCID 11678369, Verbindung

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 2.1 gm of 8-benzyl-3-[2-(4-nitrophenyl)ethyl]-1-propylxanthine (9), 1.02 gm of sodium carbonate, 3.82 ml of 1,2-dichloroethane and 0.59 ml of 2-(ethylamino)ethanol was heated in a steel pressure vessel under argon at 120 degrees C. for 3–5 hours*. The mixture was then cooled and vented to the atmosphere. The semisolid reaction mixture was triturated several times with 5–10 ml portions of methanol followed by methylene chloride and the combined solutions were evaporated to dryness. The residue was purified by column chromatography on silica gel using a gradient of 1:1 ethyl acetate-hexanes, ethyl acetate and 5% methanol in ethyl acetate. The appropriate fractions were collected and evaporated to dryness to yield a light orange solid of 8-benzyl-7-[2-ethyl(2-hydroxyethyl)amino]ethyl-3-[2-(4-nitrophenyl)ethyl]-1-propylxanthine.

Aufarbeitung

  1. waitfor 3–5 hours*
  2. temperatureThe mixture was then cooled
  3. customThe semisolid reaction mixture
  4. customwas triturated several times with 5–10 ml portions of methanol
  5. customthe combined solutions were evaporated to dryness
  6. customThe residue was purified by column chromatography on silica gel using a gradient of 1:1 ethyl acetate-hexanes, ethyl acetate and 5% methanol in ethyl acetate
  7. customThe appropriate fractions were collected
  8. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-63425db14a1b4236a40c973a03688f23
Quelldatensatz
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07247639B2

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