Trityl chloride → HCID 69748255, Verbindung

HRID 1073012Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1073012
[OH:1][CH:2]([CH2:24][OH:25])[CH2:3][O:4][C:5](=[O:23])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]/[CH:13]=[CH:14]\[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22].[C:26]1([C:32](Cl)([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>ClCCl.N1C=CC=CC=1>[OH:1][CH:2]([CH2:24][O:25][C:32]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=1)[C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1)[CH2:3][O:4][C:5](=[O:23])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]/[CH:13]=[CH:14]\[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22]

Komponenten

4

Edukt 2

HCID 6456Trityl chlorideHCID 5283468Glyceryl Monooleate

Produkt 1

HCID 69748255HCID 69748255, VerbindungAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21875418Pyridine methylene chlorideLösungsmittel

Versuchsvorschrift

A solution of 2 (21 mmol) in 80 ml of dichloromethane/pyridine (1:1) is added dropwise with triphenylmethyl chloride (27 mmol) and stirred at room temperature for 48 hours. The solvent is removed, and the residue is added twice with 50 ml of toluene and concentrated. The residue is diluted with 100 ml of H2O and extracted three times with 50 ml of dichloromethane. The combined organic phases are washed with 50 ml of cold 5% HCl and 50 ml of saturated NaCl solution, dried over MgSO4, filtrated and concentrated. The residue is purified by chromatography on silica gel using heptane/ethyl acetate (5:1). Yield: 88% of a colorless oil.

Aufarbeitung

  1. customThe solvent is removed
  2. additionthe residue is added twice with 50 ml of toluene
  3. concentrationconcentrated
  4. additionThe residue is diluted with 100 ml of H2O
  5. extractionextracted three times with 50 ml of dichloromethane
  6. washThe combined organic phases are washed with 50 ml of cold 5% HCl and 50 ml of saturated NaCl solution
  7. dry with materialdried over MgSO4
  8. filtrationfiltrated
  9. concentrationconcentrated
  10. customThe residue is purified by chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-0f8191dfe4b8477e84eed61d6690ff65
Quelldatensatz
uspto-grants-2005_06
Patentnummer
US06911553B1

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