Sodium Hydroxide → HCID 20340740, Verbindung

HRID 1076244Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1076244
O[CH2:2][CH2:3][CH2:4][C:5]1[N:13]=[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][N:7]2[N:6]=1.P(Cl)(Cl)([Cl:16])=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[Cl:16][CH2:2][CH2:3][CH2:4][C:5]1[N:13]=[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][N:7]2[N:6]=1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 20340747HCID 20340747, Verbindung

Produkt 1

HCID 20340740HCID 20340740, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a solution of 34.5g of 2-(3-hydroxypropyl)-s-triazolo-[1,5-a]pyridine in 500 ml of chloroform is added dropwise 77g of phosphorous oxychloride at a temperature of from 5° to 15°C. After the addition is completed, the reaction mixture is heated on a water bath for 1 hr. and then added to 300 g of ice-water. The mixture is then treated with an aqueous sodium hydroxide solution. Then the organic layer is separated from the aqueous layer, dried over anhydrous sodium sulfate and concentrated to give the residue, which is chromatographed over alumina with benzene. Twenty-three grams of 2-(3-chloropropyl)-s-triazolo[1,5-a]pyridine are obtained as colorless needles after recrystallization from cyclohexane, melting point 56.5°-57°C.

Aufarbeitung

  1. additionAfter the addition
  2. temperaturethe reaction mixture is heated on a water bath for 1 hr
  3. customThen the organic layer is separated from the aqueous layer
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customto give the residue, which
  7. customis chromatographed over alumina with benzene

Quellen und Nachweise

ORD-Eintrag
ord-bd3c24cddbf7480cb8229d47b53f7141
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03956328

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