Thionyl Chloride → HCID 54025343, Verbindung

HRID 1288166Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1288166
[CH2:1]([O:3][C:4]([N:6]1[CH2:20][CH2:19][C:18]2[C:9](=[N:10][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=3[C:17]=2[CH3:21])[CH:8](O)[CH2:7]1)=[O:5])[CH3:2].S(Cl)([Cl:25])=O>>[CH2:1]([O:3][C:4]([N:6]1[CH2:20][CH2:19][C:18]2[C:9](=[N:10][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=3[C:17]=2[CH3:21])[CH:8]([Cl:25])[CH2:7]1)=[O:5])[CH3:2]

Komponenten

3

Edukt 2

HCID 24386Thionyl ChlorideHCID 53875304HCID 53875304, Verbindung

Produkt 1

HCID 54025343HCID 54025343, Verbindung

Versuchsvorschrift

1 gm (3.3 millimols) of 5-hydroxy-1,2,4,5-tetrahydro-11methyl-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester was stirred for 2 hours with 20 ml of thionyl chloride at room temperature. The excess thionyl chloride was then distilled off in vacuo, the residue was dissolved in chloroform, the solution was dried with sodium sulfate, and the solvent was distilled off. After purification of the residue on a silicagel column with benzene/ethyl acetate (8:2) as the eluant, the yield was 0.55 gm (52% of theory), m.p. 131° C.

Aufarbeitung

  1. distillationThe excess thionyl chloride was then distilled off in vacuo
  2. dissolutionthe residue was dissolved in chloroform
  3. dry with materialthe solution was dried with sodium sulfate
  4. distillationthe solvent was distilled off
  5. customAfter purification of the residue on a silicagel column with benzene/ethyl acetate (8:2) as the eluant

Quellen und Nachweise

ORD-Eintrag
ord-9adbbbdbf2a241d3aad2826b7091c370
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03987047

Notizen zur Reaktion

Wird geladen…