Triphenylphosphine → HCID 67001595, Verbindung

HRID 2191582Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2191582
[C:1]([O:5][C:6](=[O:16])[NH:7][CH:8]([CH2:14][OH:15])[C:9]([CH3:13])([CH3:12])[CH2:10]O)([CH3:4])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[C:1]([O:5][C:6](=[O:16])[NH:7][CH:8]1[C:9]([CH3:13])([CH3:12])[CH2:10][O:15][CH2:14]1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 11776Triphenylphosphine2×HCID 73096807HCID 73096807, Verbindung

Produkt 1

HCID 67001595HCID 67001595, VerbindungAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

(3-Hydroxy-1-hydroxymethyl-2,2-dimethyl-propyl)-carbamic acid tert-butyl ester (104 mg, 0.44 mmol) was dissolved in dichloromethane (2.2 mL). Triphenylphosphine (0.115 g, 0.44 mmol) was added followed by azodiethylcarboxylate (0.16 mL, 0.88 mmol). After 30 min additional triphenylphosphine (0.115 g, 0.44 mmol) and azodiethylcarboxylate (0.16 mL, 0.88 mmol) were added and the reaction mixture was stirred for 72 h. The solvent was evaporated and the residue purified by silica gel chromatography (ethyl acetate/hexanes) to give 70 mg (74%) of (4,4-dimethyl-tetrahydro-furan-3-yl)-carbamic acid tert-butyl ester.

Aufarbeitung

  1. customThe solvent was evaporated
  2. customthe residue purified by silica gel chromatography (ethyl acetate/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-8944090ef8fe48e2bf7373bbd6eebcb2
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08329699B2

Notizen zur Reaktion

Wird geladen…