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Thiophosgene → HCID 13563671, Verbindung

HRID 979720
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 979720
[C:1]([C:5]1[CH:6]=[C:7]([OH:12])[CH:8]=[CH:9][C:10]=1[Cl:11])([CH3:4])([CH3:3])[CH3:2].[C:13](Cl)([Cl:15])=[S:14].[OH-].[Na+]>C(Cl)(Cl)Cl>[Cl:15][C:13]([O:12][C:7]1[CH:8]=[CH:9][C:10]([Cl:11])=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH:6]=1)=[S:14]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 10040ThiophosgeneHCID 14798Sodium HydroxideHCID 109102303-Tert-butyl-4-chlorophenol

Produkt 1

HCID 13563671HCID 13563671, VerbindungAusbeute 72,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

Into 50 ml of chloroform were dissolved 9.2 g of 3-tert-butyl-4-chlorophenol and 6.3 g of thiophosgene, and 60 ml of 1N-sodium hydroxide solution were added dropwise thereto with stirring at room temperature. After completion of this dropwise addition, the mixture was subjected to stirring over a period of 3 hours. From the reaction mixture was separated chloroform layer, which was thereafter dried over anhydrous calcium chloride. Then, chloroform was distilled off and the residue was distilled under reduced pressure to give 9.5 g of O-3-tert-butyl-4-chlorophenyl chlorothioformate having boiling point of 103°-106° C./0.5 mmHg, of which properties are as follows.

Aufarbeitung

  1. additionwere added dropwise
  2. additionAfter completion of this dropwise addition
  3. stirringto stirring over a period of 3 hours
  4. customFrom the reaction mixture was separated chloroform layer, which
  5. dry with materialwas thereafter dried over anhydrous calcium chloride
  6. distillationThen, chloroform was distilled off
  7. distillationthe residue was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7e9adeac2b2140798021751f2df1614a
Quelldatensatz
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04668831

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