Hydrochloric Acid → HCID 15227821, Verbindung

HRID 1440322Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1440322
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:13]=[C:12]([C:14](=[O:17])[CH2:15][CH3:16])[O:11][N:10]=2)=[CH:5][CH:4]=1.[CH2:18]=O.[NH:20]1[CH2:24][CH2:23][CH2:22][CH2:21]1.Cl>C(OCC)C.O.ClCCl.C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:13]=[C:12]([C:14](=[O:17])[CH:15]([CH3:18])[CH2:16][N:20]3[CH2:24][CH2:23][CH2:22][CH2:21]3)[O:11][N:10]=2)=[CH:7][CH:8]=1

Komponenten

9

Edukt 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 31268PyrrolidineHCID 19976958HCID 19976958, Verbindung

Produkt 1

HCID 15227821HCID 15227821, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Added to a mixed solvent of 22 ml of ethyl alcohol and 5 ml of dichloromethane were 2.22 g (9.61 mmol) of 3-(4-methoxyphenyl)-5-propionylisoxazole, 0.96 ml of a 37% aqueous formaldehyde solution and 1.37 g (19.2 mmol) of pyrrolidine, followed by stirring at room temperature for 8 hours. Water and ethyl ether were added, and the resultant mixture was acidified with 2N-hydrochloric acid. The water layer was separated and collected. After the water layer was alkalinized with an aqueous solution of potassium hydroxide, dichloromethane was added for extraction. The solvent was distilled off, whereby 3-(4-methoxyphenyl)-5-{2-methyl-3-(1-pyrrolidinyl)propionyl}isoxazole was obtained as colorless crystals.

Aufarbeitung

  1. customThe water layer was separated
  2. customcollected
  3. additionwas added for extraction
  4. distillationThe solvent was distilled off

Quellen und Nachweise

ORD-Eintrag
ord-0f001247b815491abfc3fbdcde365af8
Quelldatensatz
uspto-grants-1996_03
Patentnummer
US05498619

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