Glycolic Acid → HCID 20439386, Verbindung

HRID 1979536Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1979536
I.[NH2:2][NH:3][C:4]([NH:23][CH3:24])=[N:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH:11]=1.[C:25](O)(=O)[CH2:26][OH:27]>C1C=CC=CC=1>[CH3:24][N:23]1[C:4]([NH:5][CH2:6][CH2:7][CH2:8][O:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([CH2:16][N:17]3[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]3)[CH:11]=2)=[N:3][N:2]=[C:25]1[CH2:26][OH:27]

Komponenten

4

Edukt 2

HCID 757Glycolic AcidHCID 178484962HCID 178484962, Verbindung

Produkt 1

HCID 20439386HCID 20439386, VerbindungAusbeute 0,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

N-Amino-N'-methyl-N"-[3-[3-(1-piperidinylmethyl)phenoxy]propyl]guanidine hydroiodide (2.24 g) and glycolic acid (1.52 g) were heated together for 3 h in dry benzene (25 ml) at reflux. The benzene was decanted from the residual oil, which was partitioned between ethyl acetate and aqueous 1N sodium hydroxide solution. The organic phase was chromatographed on silica using methanol to give a white solid. This solid was washed with boiling ethyl acetate to leave the title compound as a white solid (0.013 g) m.p. 151°-2°.

Aufarbeitung

  1. temperatureat reflux
  2. customThe benzene was decanted from the residual oil, which
  3. customwas partitioned between ethyl acetate and aqueous 1N sodium hydroxide solution
  4. customThe organic phase was chromatographed on silica
  5. customto give a white solid
  6. washThis solid was washed with boiling ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-925bfb0cf0f04e77b078278809814672
Quelldatensatz
uspto-grants-1984_11
Patentnummer
US04481199

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