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Phosphorus oxychloride → HCID 19043054, Verbindung

HRID 1683195
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1683195
C(NCC[C:6]1[C:11]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:10]=2[CH:9]=[CH:8][CH:7]=1)=O.P(Cl)(Cl)(Cl)=O.[CH3:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([S:30]([CH2:33][CH3:34])(=[O:32])=[O:31])=[CH:26][C:25]=1[C:35]1[NH:36][CH:37]=[CH:38][CH:39]=1.[BH4-].[Na+]>ClCCCl.O.CO>[C:6]1([N:36]([CH2:37][C:37]2[NH:36][C:35]([C:25]3[CH:26]=[C:27]([S:30]([CH2:33][CH3:34])(=[O:31])=[O:32])[CH:28]=[CH:29][C:24]=3[O:23][CH3:22])=[CH:39][CH:38]=2)[CH2:35][CH3:25])[C:11]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:10]=2[CH:9]=[CH:8][CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 24813Phosphorus oxychlorideHCID 4311764Sodium borohydrideHCID 139003532-[5-(Ethanesulfonyl)-2-methoxyphenyl]-1H-pyrroleHCID 86750935HCID 86750935, Verbindung

Produkt 1

HCID 19043054HCID 19043054, VerbindungAusbeute 207,2 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 11
1,2-Dichloroethane
Lösungsmittel
2×
HCID 887MethanolLösungsmittel
HCID 962WaterLösungsmittel2×

Versuchsvorschrift

N-Formyl-N-(benzocycloheptan-1-yl)ethylamine (0.39 g, 1.81 mmol) was treated with phosphorus oxychloride (0.17 ml, 1.81 mmol) at room temperature under argon. After 30 minutes, 1,2-dichloroethane (1.2 ml) was added at 0° C. followed by a solution of 2-(2-methoxy-5-ethylsulfonylphenyl)-1H-pyrrole (0.4 g, 1.51 mmol) in 1,2-dichloroethane (4 ml). The mixture was allowed to warm to room temperature and stirred for 16 h at 25° C. and then for 6 h at 40° C. Sodium borohydride (0.55 g, 14.5 mmol) was then added at 0° C., and the reaction mixture was warmed to room temperature and stirred for 3 h. Water (2.4 ml) and then methanol (2.4 ml) were added dropwise. More water (30 ml) was added and the borane complex was extracted with dichloromethane (3×30 ml). The combined organics were dried (Na2SO4) and evaporated to an oil which was then treated with methanol (4.8 ml) and conc. HCl (2.4 ml) at room temperature for 16 h. The mixture was diluted with water (25 ml) and basified with 40% aqueous NaOH. Extraction into dichloromethane (3×30 ml), followed by drying (Na2SO4) and evaporation of the organic extracts gave an orange oil (0.73 g). The crude material was purified by chromatography on silica eluting with ethyl acetate (20-50%)--hexane, to give the title compound as an orange oil (0.31 g, 44%)

Aufarbeitung

  1. waitfor 6 h at 40° C
  2. temperaturethe reaction mixture was warmed to room temperature
  3. stirringstirred for 3 h
  4. extractionthe borane complex was extracted with dichloromethane (3×30 ml)
  5. dry with materialThe combined organics were dried (Na2SO4)
  6. customevaporated to an oil which
  7. additionwas then treated with methanol (4.8 ml) and conc. HCl (2.4 ml) at room temperature for 16 h
  8. additionThe mixture was diluted with water (25 ml)
  9. extractionExtraction into dichloromethane (3×30 ml)
  10. customby drying
  11. custom(Na2SO4) and evaporation of the organic extracts

Quellen und Nachweise

ORD-Eintrag
ord-edaa01d2f61948dd80950de85b8fcbc5
Quelldatensatz
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05637609

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