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1-(2-Hydroxyethyl)piperazine → 1-(3-(Di(tert-butyldimethylsiloxy)-methyl-silanyl)-propoxy)-3-(4-(2-hydroxy-ethyl)-piperidin-1-yl)-propan-2-ol

HRID 1261467
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1261467
[N:1]1([CH2:7][CH2:8][OH:9])[CH2:6][CH2:5]N[CH2:3][CH2:2]1.[C:10]([Si:14]([CH3:34])([CH3:33])[O:15][Si:16]([CH:26]([CH2:29][CH:30]1[CH2:32][O:31]1)CC)([CH3:25])[O:17][Si:18]([C:21]([CH3:24])([CH3:23])[CH3:22])([CH3:20])[CH3:19])([CH3:13])([CH3:12])[CH3:11]>C(O)C>[O:15]([Si:16]([O:17][Si:18]([C:21]([CH3:24])([CH3:23])[CH3:22])([CH3:20])[CH3:19])([CH3:25])[CH2:26][CH2:29][CH2:30][O:31][CH2:32][CH:8]([OH:9])[CH2:7][N:1]1[CH2:6][CH2:5][CH:26]([CH2:29][CH2:30][OH:31])[CH2:3][CH2:2]1)[Si:14]([C:10]([CH3:11])([CH3:13])[CH3:12])([CH3:34])[CH3:33]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 76771-(2-Hydroxyethyl)piperazineHCID 866322801,5-Di(tert-butyl)-3-(oxiranylmethylpropyl)-1,1,3,5,5-Pentamethyltrisiloxane

Produkt 1

HCID 668726811-(3-(Di(tert-butyldimethylsiloxy)-methyl-silanyl)-propoxy)-3-(4-(2-hydroxy-ethyl)-piperidin-1-yl)-propan-2-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

2-piperazin-1-yl-ethanol (0.61 g) and ethanol (20 mL) were charged to a 100 mL RB flask equipped with a magnetic stirrer. The mixture was stirred and heated to 70° C. 1,5-Di(tert-butyl)-3-(oxiranylmethylpropyl)-1,1,3,5,5-Pentamethyltrisiloxane (2.0 g) was placed in an addition funnel and added dropwise to the flask. The mixture was stirred and maintained at 70° C. for an additional 4 hours. The reaction progress was monitored by NMR spectroscopy. Upon reaction completion, the ethanol was removed by rotovap, and the mixture was distilled under reduced pressure to remove impurities.

Aufarbeitung

  1. customequipped with a magnetic stirrer
  2. additionadded dropwise to the flask
  3. stirringThe mixture was stirred
  4. temperaturemaintained at 70° C. for an additional 4 hours
  5. customUpon reaction completion
  6. customthe ethanol was removed by rotovap
  7. distillationthe mixture was distilled under reduced pressure
  8. customto remove impurities

Quellen und Nachweise

ORD-Eintrag
ord-7bccf76ea9af49fca9f4025889cfe387
Quelldatensatz
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08470894B2

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