Water → HCID 20222067, Verbindung

HRID 980123Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 980123
[CH2:1]([O:3][C:4]([C:6]1[CH:15]=[C:14]([OH:16])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]=1[OH:17])=[O:5])[CH3:2].S(Cl)([Cl:21])(=O)=O.O>C(Cl)(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[C:7](=[O:17])[C:8]2[C:13]([C:14](=[O:16])[C:15]=1[Cl:21])=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:5])[CH3:2]

Komponenten

5

Edukt 3

HCID 962WaterHCID 24648Sulfuryl chlorideHCID 12388086Ethyl 1,4-dihydroxynaphthalene-2-carboxylate

Produkt 1

HCID 20222067HCID 20222067, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

23 g of compound (6) prepared above was suspended in 300 ml of chloroform and, while keeping the solution at 5°-10° C., 27.4 g of sulfuryl chloride was slowly dropwise added thereto. After reacting for 1.5 hours, water was added to the reaction solution to conduct separation and extraction. The organic phase was dried with anhydrous sodium sulfate, and chloroform was distilled off under reduced pressure. Rapid purification of the residue through silica gel column chromatography gave compound (7) as crystals. Yield: 8.8 g (33%).

Aufarbeitung

  1. customat 5°-10° C.
  2. customseparation and extraction
  3. dry with materialThe organic phase was dried with anhydrous sodium sulfate, and chloroform
  4. distillationwas distilled off under reduced pressure
  5. customRapid purification of the residue through silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-5dbe7fa807994653afa3cb482d6162ca
Quelldatensatz
uspto-grants-1987_01
Patentnummer
US04636456

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