Phosphorus sulfide (P2S5) → 8-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

HRID 247278

Reaktionsgleichung

Reaktionsgleichung von HRID 247278
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=O)[N:7]([CH3:14])[CH2:8][CH:9]([CH2:11][CH2:12][Cl:13])[O:10][C:4]=2[CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19].[S-2].[K+].[K+]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6](=[S:19])[N:7]([CH3:14])[CH2:8][CH:9]([CH2:11][CH2:12][Cl:13])[O:10][C:4]=2[CH:3]=1

Komponenten

5

Edukt 3

HCID 14817Phosphorus sulfide (P2S5)HCID 162263Potassium SulfideHCID 137262948-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one

Produkt 1

HCID 137262998-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thioneAusbeute 73,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a solution of 43 g (0.16 mole) of 8-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in 400 ml of dry toluene was added a mixture of 23 g (0.12 mole) of phosphorus pentasulfide and 23 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux for 24 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure to give 25.5 g (55%) of orange oil which solidified on standing at room temperature. The solid was recrystallized from ethanol, m.p. 105°-106° C.

Aufarbeitung

  1. temperatureheated
  2. temperatureat reflux for 24 hr
  3. filtrationThe mixture was filtered hot
  4. concentrationthe filtrate concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-11a7691106584167a71465ffbdf88a60
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04705853

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