Phosphorus sulfide (P2S5) → 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepine-2-thione

HRID 1580643Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1580643
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=O)[CH:9]([CH3:13])[N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[S:22])[CH:9]([CH3:13])[N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1

Komponenten

4

Edukt 2

HCID 14817Phosphorus sulfide (P2S5)HCID 382377-chloro-3-methyl-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepin-2-one

Produkt 1

HCID 126124347-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepine-2-thione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A stirred mixture of 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one (0.294 mole), dry pyridine (2300 ml.) and phosphorus pentasulfide (72.4 g.; 0.323 mole) is reflexed under nitrogen for 30 minutes, cooled and concentrated in vacuo. A suspension of the residue in ice water is extracted with methylene chloride. The extract is dried over anhydrous potassium carbonate and concentrated. The residue thus obtained is crystallized from methylene chlorideethanol to give 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepine-2-thione.

Aufarbeitung

  1. temperaturecooled
  2. concentrationconcentrated in vacuo
  3. additionA suspension of the residue in ice water
  4. extractionis extracted with methylene chloride
  5. dry with materialThe extract is dried over anhydrous potassium carbonate
  6. concentrationconcentrated
  7. customThe residue thus obtained
  8. customis crystallized from methylene chlorideethanol

Quellen und Nachweise

ORD-Eintrag
ord-98251a72024043dba100ede69d665bbb
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03933794

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