Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 21024036, Verbindung

HRID 1795689Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1795689
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.[Cl:18][CH2:19][C:20]([O:22][CH:23]1[C:24]([O:66]C(OCC)C)([CH3:65])[CH2:25][CH2:26][CH:27]([O:59]C(OCC)C)[CH2:28][C:29]([O:31][CH:32](/[C:37](/[CH3:58])=[CH:38]/[CH:39]=[CH:40]/[CH:41]([CH3:57])[CH2:42][CH:43]2[O:56][CH:44]2[CH:45]([CH3:55])[CH:46]([O:49]C(OCC)C)[CH2:47][CH3:48])[CH:33]([CH3:36])[CH:34]=[CH:35]1)=[O:30])=[O:21]>CO>[Cl:18][CH2:19][C:20]([O:22][CH:23]1[C:24]([OH:66])([CH3:65])[CH2:25][CH2:26][CH:27]([OH:59])[CH2:28][C:29]([O:31][CH:32](/[C:37](/[CH3:58])=[CH:38]/[CH:39]=[CH:40]/[CH:41]([CH3:57])[CH2:42][CH:43]2[O:56][CH:44]2[CH:45]([CH3:55])[CH:46]([OH:49])[CH2:47][CH3:48])[CH:33]([CH3:36])[CH:34]=[CH:35]1)=[O:30])=[O:21]

Komponenten

4

Edukt 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 21024035HCID 21024035, Verbindung

Produkt 1

HCID 21024036HCID 21024036, VerbindungAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Pyridinium p-toluenesulfonate (1 mg, 4.1 μmol) was added to a solution of (8E,12E,14E)-7-chloroacetoxy-3,6,21-tri(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide (3.2 mg, 4.06 μmol) in methanol (1 mL), followed by stirring at room temperature for one hour. The reaction solution was evaporated, and the resulting residue was purified by thin layer chromatography (MERCK Silica gel 60 F254, 0.2 mm, developing solution; ethyl acetate-hexane=2:1) to obtain the title compound (1.6 mg, 70%) as a colorless oil.

Aufarbeitung

  1. customThe reaction solution was evaporated
  2. customthe resulting residue was purified by thin layer chromatography (MERCK Silica gel 60 F254, 0.2 mm, developing solution; ethyl acetate-hexane=2:1)

Quellen und Nachweise

ORD-Eintrag
ord-b1893cbd9d8e4068a07772c5bcf37a48
Quelldatensatz
uspto-grants-2006_04
Patentnummer
US07026352B1

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