Water → 2-Isothiocyanato-3-phenylpyridine

HRID 1287485Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1287485
[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[Ca+2].O.[C:20](Cl)(Cl)=[S:21]>CCOCC>[C:8]1([C:7]2[C:2]([N:1]=[C:20]=[S:21])=[N:3][CH:4]=[CH:5][CH:6]=2)[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 27627953-Phenylpyridin-2-amine

Produkt 1

HCID 215089042-Isothiocyanato-3-phenylpyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

6 G. of 2-amino-3-phenylpyridine and 7.4 g. of calcium carbonate in 500 ml. of water is added to a solution of 2.9 ml. thiophosgene in 105 ml. of ether. The reaction mixture is stirred at room temperature for 3 hours and the ether layer is separated. The water layer is extracted with ether and the combined ether extracts dried and evaporated to dryness affording 3-phenyl-2-pyridylisothiocyanate. The residue from the evaporation is allowed to stand at room temperature for 3 days. The reaction mixture is then triturated with ether and filtered affording 9-phenyl-3-(3-phenyl-2-pyridyl) pyrido (1,2-a) 1,3,5-triazine-2,4-dithione m.p. 90°-92° C.

Aufarbeitung

  1. customthe ether layer is separated
  2. extractionThe water layer is extracted with ether
  3. dry with materialthe combined ether extracts dried
  4. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-10d1e4cac73343dc8e3f9a8ca2b27575
Quelldatensatz
uspto-grants-1976_10
Patentnummer
US03984549

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