Thionyl Chloride → HCID 21430653, Verbindung

HRID 437200Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 437200
C([O:3][C:4]([C:6]1[O:7][C:8]2[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH2:18][CH:19](O)[CH2:20][O:21][C:22]3[C:27]4[C:28](=[O:37])[CH:29]=[C:30]([C:32]([O:34]CC)=[O:33])[O:31][C:26]=4[CH:25]=[CH:24][CH:23]=3)[C:9]=2[C:10](=[O:12])[CH:11]=1)=[O:5])C.S(Cl)([Cl:41])=O>ClCCCl>[Cl:41][CH:19]([CH2:20][O:21][C:22]1[C:27]2[C:28](=[O:37])[CH:29]=[C:30]([C:32]([OH:34])=[O:33])[O:31][C:26]=2[CH:25]=[CH:24][CH:23]=1)[CH2:18][O:17][C:13]1[C:9]2[C:10](=[O:12])[CH:11]=[C:6]([C:4]([OH:3])=[O:5])[O:7][C:8]=2[CH:16]=[CH:15][CH:14]=1

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 204318Cromophene

Produkt 1

HCID 21430653HCID 21430653, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

A mixture of 24.5 parts of 5,5'-[(2-hydroxytrimethylene)dioxy]bis [4-oxo-4H-1-benzopyran-2-carboxylic acid] diethyl ester and 47.6 parts of thionyl chloride in 40 parts of dry 1,2-dichloroethane was refluxed for 16 hours. The solvent was then evaporated, the residue was triturated with petrol and the resulting solid was crystallized from ethanol to give 15.6 parts of 5,5'-[(2-chlorotrimethylene)dioxy]bis[4-oxo-4H-1-benzopyran-2-carboxylic acid], diethyl ester as white crystals m.p. 144°-144.5° C.

Aufarbeitung

  1. temperaturewas refluxed for 16 hours
  2. customThe solvent was then evaporated
  3. customthe residue was triturated with petrol
  4. customthe resulting solid was crystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-cd0b45c5018846c6a64979c86d933310
Quelldatensatz
uspto-grants-1977_06
Patentnummer
US04029802

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