1-Pyrrolidineethanol → 2-[N-Pyrollidinyl]ethyl Tributylstannyl Ether

HRID 65559

Reaktionsgleichung

Reaktionsgleichung von HRID 65559
CCCC[Sn]([O:14][Sn:15]([CH2:24][CH2:25][CH2:26][CH3:27])([CH2:20][CH2:21][CH2:22][CH3:23])[CH2:16][CH2:17][CH2:18][CH3:19])(CCCC)CCCC.O[CH2:29][CH2:30][N:31]1[CH2:35][CH2:34][CH2:33][CH2:32]1>C1C=CC=CC=1>[CH2:24]([Sn:15]([O:14][CH2:29][CH2:30][N:31]1[CH2:35][CH2:34][CH2:33][CH2:32]1)([CH2:16][CH2:17][CH2:18][CH3:19])[CH2:20][CH2:21][CH2:22][CH3:23])[CH2:25][CH2:26][CH3:27]

Komponenten

4

Edukt 2

HCID 762881-PyrrolidineethanolHCID 16682746Bis(tributyltin) oxide

Produkt 1

HCID 227570402-[N-Pyrollidinyl]ethyl Tributylstannyl Ether

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

2-[N-Pyrollidinyl]ethyl Tributylstannyl Ether is prepared from 65.0 gm (.109 mole) bis(tributyltin) oxide and 25.0 gm (.217 mole) N-(β-hydroxyethyl)pyrolidine in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After refluxing 20 hours, a total of 2.0 ml of water (theory 1.96 ml) had collected in the Dean-Starke tube. The solvent is stripped off on a rotating evaporator to provide 94.0 gm of yellow liquid. This is fractionated at reduced pressure with collection at 150°-154° C. at 0.3 mm of water-white liquid (Percent yield - 63). Infrared spectral analysis shows this liquid to be the desired ether.

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux in a system that
  3. temperatureAfter refluxing 20 hours
  4. customa total of 2.0 ml of water (theory 1.96 ml) had collected in the Dean-Starke tube
  5. customThe solvent is stripped off on a rotating evaporator

Quellen und Nachweise

ORD-Eintrag
ord-8cdb46d0b3cd42f2b60bc4555b228118
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04128429

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