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Imidazole → Triphenylphosphine Oxide

HRID 533512
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 533512
[C:1]1([P:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1C=CN=C1.[I:25]I.[Br:27][C:28]1[CH:33]=[CH:32][C:31]([CH2:34][CH2:35][OH:36])=[C:30]([CH3:37])[CH:29]=1>ClCCl>[C:14]1([P:7](=[O:36])([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1.[Br:27][C:28]1[CH:33]=[CH:32][C:31]([CH2:34][CH2:35][I:25])=[C:30]([CH3:37])[CH:29]=1
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Komponenten

7

Edukt 4

HCID 795ImidazoleHCID 807IodineHCID 11776TriphenylphosphineHCID 578428522-(4-Bromo-2-methylphenyl)ethanol

Produkt 2

HCID 13097Triphenylphosphine OxideHCID 665779234-Bromo-1-(2-iodo-ethyl)-2-methyl-benzene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a 250 mL flask in an ice bath was added triphenyl phosphine (6.17 g, 22.8 mmol), imidazole (1.6 g, 22.8 mmol) and 100 mL of anhydrous dichloromethane. Once dissolved, iodine (5.79 g, 22.8 mmol) was added. The reaction was then stirred for about 30 minutes (ppt formed). The 2-(4-bromo-2-methylphenyl)ethanol (3.93 g, 18.3 mmol) was added in batches and the flask was rinsed with the remaining DCM (22 mL) which was also added to the reaction mixture. The reaction was warmed to room temperature and was stirred overnight. The reaction mixture was filtered through a small pad of celite and washed with DCM (100 mL). The filtrate was washed with saturated aqueous sodium thiosulfate (200 mL) and brine 200 mL. The organics were concentrated in vacuo to furnish a white solid (triphenyphosphine oxide+desired product). The material was triturated with heptanes for 5-10 mins then filtered to remove the majority of the triphenylphosphine oxide The filtrate was concentrated in vacuo to furnish a total of 5.86 g (98.8%) of the title compound as a clear oil that solidified upon standing. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 2.30 (s, 3H) 3.04-3.20 (m, 2H) 3.21-3.39 (m, 2H) 7.02 (d, J=8.20 Hz, 1H) 7.23-7.29 (m, 1H) 7.30-7.38 (m, 1H).

Aufarbeitung

  1. dissolutionOnce dissolved
  2. custom(ppt formed)
  3. washthe flask was rinsed with the remaining DCM (22 mL) which
  4. additionwas also added to the reaction mixture
  5. stirringwas stirred overnight
  6. filtrationThe reaction mixture was filtered through a small pad of celite
  7. washwashed with DCM (100 mL)
  8. washThe filtrate was washed with saturated aqueous sodium thiosulfate (200 mL) and brine 200 mL
  9. concentrationThe organics were concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3c64bb31a0aa4df389a268d4e948e960
Quelldatensatz
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08853258B2

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