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HRID 4811Erstellt: 24. Oktober 2026

Phosphorus sulfide (P2S5) → 2-(2-Chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepine-5(4H)-thione

https://huagongshe.com/de/reaction/4811

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktPhosphorus sulfide (P2S5)HCID 14817—
EduktPotassium SulfideHCID 162263—
Edukt2-(2-Chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepin-5(4H)-oneHCID 13726297—
LösungsmittelChloroformHCID 6212—
Produkt2-(2-Chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepine-5(4H)-thioneHCID 1372630286,3%

Reaktionsschritte

To a solution of 10.3 g (0.04 mole) of 2-(2-chloroethyl)-2,3-dihydro-7-methoxy-4-methyl-1,4-benzoxazepin-5(4H)-one in 200 ml of chloroform was added a mixture of 5.7 g (0.03 mole) of phosphorus pentasulfide and 5.7 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux under nitrogen atmosphere for 5 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure. The residue, an orange solid, was recrystallized from ethanol to give 7.4 g (65%) of product, m.p. 98°-100° C.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS04727152
Quelldatensatzuspto-grants-1988_02
ORD IDord-ffbaf1c2ea5949e094d1b0c62e55de55
Quellennotizuspto-grants-1988_02