Tetrachlorobisphenol A → 2-(3,5-Dichloro-4-hydroxyphenyl)-2-(3,5-dichloro-4-cyanatophenyl)-propane

HRID 1439534

Reaktionsgleichung

Reaktionsgleichung von HRID 1439534
[Cl:1][C:2]1[CH:3]=[C:4]([C:10]([C:13]2[CH:18]=[C:17]([Cl:19])[C:16]([OH:20])=[C:15]([Cl:21])[CH:14]=2)([CH3:12])[CH3:11])[CH:5]=[C:6]([Cl:9])[C:7]=1[OH:8].[N:22]#[C:23]Cl.C([O-])([O-])=O.[Na+].[Na+].[OH-].[Na+]>O.C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([C:10]([C:13]2[CH:18]=[C:17]([Cl:19])[C:16]([O:20][C:23]#[N:22])=[C:15]([Cl:21])[CH:14]=2)([CH3:12])[CH3:11])[CH:5]=[C:6]([Cl:9])[C:7]=1[OH:8]

Komponenten

7

Edukt 4

HCID 6619Tetrachlorobisphenol AHCID 10340Sodium CarbonateHCID 10477Cyanogen ChlorideHCID 14798Sodium Hydroxide

Produkt 1

HCID 213958592-(3,5-Dichloro-4-hydroxyphenyl)-2-(3,5-dichloro-4-cyanatophenyl)-propaneAusbeute 99,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

36.6 g (0.1 mol) of 2,2-bis-(3,5-dichloro-4-hydroxyphenyl)-propane are suspended in 500 ml of water and 400 ml of methylene chloride. After cooling to about 0° to 3° C, 20 ml (0.4 mol) of cyanogen chloride are added. A solution of 10.6 g of Na2CO3 in 50 ml of water is added dropwise over the course of 90 minutes, with vigorous stirring, in such a way that the pH value of the reaction mixture is constantly kept in the range between 7.5 and 8.5. Thereafter, 1 N NaOH is added in such a way that a pH value of the reaction mixture of about 8.0 is maintained, and persists as the final value. Thereafter, the organic phase is separated off, washed with 100 ml of water and concentrated at room temperature. 39 g (99% of theory) of 2-(3,5-dichloro-4-hydroxyphenyl)-2-(3,5-dichloro-4-cyanatophenyl)-propane are obtained as the residue.

Aufarbeitung

  1. temperatureAfter cooling to about 0° to 3° C
  2. additionthat a pH value of the reaction mixture of about 8.0
  3. temperatureis maintained
  4. customThereafter, the organic phase is separated off
  5. washwashed with 100 ml of water
  6. concentrationconcentrated at room temperature

Quellen und Nachweise

ORD-Eintrag
ord-13f3c81c6ca146db9978f7c0560d11dd
Quelldatensatz
uspto-grants-1977_11
Patentnummer
US04060541

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