Diethyl Ether → HCID 1415664, Verbindung

HRID 615103Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 615103
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[C:6](=O)([O-])[O-].[K+].[K+].CCO[CH2:15][CH3:16].[CH2:17](Br)[C:18]#[CH:19]>O>[CH2:17]([N:5]([CH2:6][C:15]#[CH:16])[C:1]([CH3:4])([CH3:3])[CH3:2])[C:18]#[CH:19]

Komponenten

6

Edukt 4

HCID 3283Diethyl EtherHCID 6385Tert-ButylamineHCID 7842Propargyl bromideHCID 11430Potassium Carbonate

Produkt 1

HCID 1415664HCID 1415664, VerbindungAusbeute 45 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 0.15 mole of t-butylamine, 0.35 mole of anhydrous, powdered potassium carbonate and 250 moles of ether was stirred mechanically and 0.25 mole of propargylbromide was added dropwise. The mixture was refluxed for about 10 hours. Water was added to dissolve the salt. The ether layer was separated and the aqueous layer was extracted twice with ether. The combined ether solution was dried over anhydrous MgSO4. The dipropargyl-t-butylamine produced was distilled at 63°-65° C./20 mm Hg to yield a yellowish liquid in a 45% yield: IR 3300, 3100, 2980 and 2940 cm-1 ; NMR (CDCl3)δ1.10, 2.20 and 3.45.

Aufarbeitung

  1. temperatureThe mixture was refluxed for about 10 hours
  2. dissolutionto dissolve the salt
  3. customThe ether layer was separated
  4. extractionthe aqueous layer was extracted twice with ether
  5. dry with materialThe combined ether solution was dried over anhydrous MgSO4

Quellen und Nachweise

ORD-Eintrag
ord-619fe9d62bc942ba8196281b4b06560f
Quelldatensatz
uspto-grants-1985_02
Patentnummer
US04497727

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