Ethanol → HCID 66672783, Verbindung

HRID 352171Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 352171
S(Cl)([Cl:3])=O.[NH2:5][CH:6]1[CH2:11][CH2:10][CH:9]([C:12]([OH:14])=[O:13])[CH2:8][CH2:7]1.[CH2:15](O)[CH3:16]>>[ClH:3].[NH2:5][CH:6]1[CH2:11][CH2:10][C:9]([CH2:15][CH3:16])([C:12]([OH:14])=[O:13])[CH2:8][CH2:7]1

Komponenten

4

Versuchsvorschrift

Thionyl chloride (2.55 mL, 35 mmol) was added dropwise to absolute ethanol (100 mL) under a N2 atmosphere. The resulting solution was stirred at room temperature for 10 min then 4-amino-1-cyclohexanecarboxylic acid (4.29 g, 30 mmol, cis, trans mixture) was added as a solid. The resulting solution was stirred at room temperature overnight. The solvent was removed in vacuo, the residue dissolved in ethanol (25 mL) and this solution was slowly added to a flask containing rapidly stirred ether (700 mL). The precipitate that formed was collected by filtration and dried in vacuo to give 5.75 g, 92% as a white solid. MS (ion spray) 172 (M+1).

Aufarbeitung

  1. stirringThe resulting solution was stirred at room temperature overnight
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue dissolved in ethanol (25 mL)
  4. additionthis solution was slowly added to a flask
  5. additioncontaining rapidly stirred ether (700 mL)
  6. customThe precipitate that formed
  7. filtrationwas collected by filtration
  8. customdried in vacuo
  9. customto give 5.75 g, 92% as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-e5e95f6eeb264a658c26157bef3f9ae0
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06743794B2

Notizen zur Reaktion

Wird geladen…