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Phosphorus oxychloride → HCID 58305987, Verbindung

HRID 2088687
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2088687
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([O:8][C:9](=[O:35])[CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([C:17]2[N:25]=[C:24]3[N:19]([C:20](=O)[NH:21][C:22]([C:26]4[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][C:27]=4[Cl:33])=[CH:23]3)[N:18]=2)[CH2:13][CH2:12]1)[CH3:7]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[CH2:6]([O:8][C:9](=[O:35])[CH2:10][N:11]1[CH2:12][CH2:13][CH:14]([C:17]2[N:25]=[C:24]3[N:19]([C:20]([Cl:3])=[N:21][C:22]([C:26]4[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][C:27]=4[Cl:33])=[CH:23]3)[N:18]=2)[CH2:15][CH2:16]1)[CH3:7]
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Komponenten

4

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 136104186Ethyl {4-[7-(2,4-dichlorophenyl)-5-oxo-5,6-dihydro[1,2,4]triazolo[1,5-c]pyrimidin-2-yl]piperidin-1-yl}acetate

Produkt 1

HCID 58305987HCID 58305987, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 66133Benzyl triethylammonium chlorideKatalysator

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

5 ml of phosphoryl chloride were added to 500 mg (1.11 mmol) of ethyl{4-[7-(2,4-dichlorophenyl)-5-oxo-5,6-dihydro [1,2,4]triazolo[1,5-c]-pyrimidin-2-yl]piperidin-1-yl}acetate (Example 54A), 1.01 g (4.44 mmol) of benzyltriethylammonium chloride were added and the reaction mixture was stirred at 120° C. for 2.5 h. The reaction mixture was concentrated and carefully, with vigorous stirring, added to saturated aqueous sodium bicarbonate solution. The pH was adjusted to pH=7 by addition of solid sodium bicarbonate. The aqueous phase was extracted three times with dichloromethane. The combined organic phases were washed once with water, dried with magnesium sulfate and then freed from the solvent. Without further purification, this gave 506 mg (88% of theory) of the product.

Aufarbeitung

  1. additionwere added
  2. concentrationThe reaction mixture was concentrated
  3. additioncarefully, with vigorous stirring, added to saturated aqueous sodium bicarbonate solution
  4. additionThe pH was adjusted to pH=7 by addition of solid sodium bicarbonate
  5. extractionThe aqueous phase was extracted three times with dichloromethane
  6. washThe combined organic phases were washed once with water
  7. dry with materialdried with magnesium sulfate
  8. customWithout further purification

Quellen und Nachweise

ORD-Eintrag
ord-ffdb0c00752c4fbeb20f7d1f543016be
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08436003B2

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