Reaktion #64851

ord-8b5de020a416400d905809c3a15a3aa5

Reaktionsgleichung

[Al+3].[H-].[H-].[H-].[H-].[Li+]
Aluminum lithium hydride
COc1ccc2c(c1)C(=O)NCCS2
7-methoxy-5-oxo-2,3,4,5-tetrahydro-1,4-benzothiazepine
O=S(=O)([O-])[O-].[Na+].[Na+]
sodium sulfate
→
COc1ccc2c(c1)CNCCS2
7-methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine
Ausbeute 94.3%

Edukte

[Al+3].[H-].[H-].[H-].[H-].[Li+]
Aluminum lithium hydride
COc1ccc2c(c1)C(=O)NCCS2
7-methoxy-5-oxo-2,3,4,5-tetrahydro-1,4-benzothiazepine
O=S(=O)([O-])[O-].[Na+].[Na+]
sodium sulfate

Reagenzien

Keine

Lösungsmittel

C1CCOC1
THF

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturat reflux for 3 hours
  3. 3
    Filtration10 hydrates, a celite filtration
  4. 4
    EinengenThe resulting filtrate was concentrated

Vorschrift

Aluminum lithium hydride (2.739) and the abovementioned 7-methoxy-5-oxo-2,3,4,5-tetrahydro-1,4-benzothiazepine (5.0 g) were added to THF (150 ml) under ice cooling and heated at reflux for 3 hours. After adding an excess amount of sodium sulfate.10 hydrates, a celite filtration was made. The resulting filtrate was concentrated to give 7-methoxy-2,3,4,5-tetrahydro-1,4-benzothiazepine (4.4 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05416066uspto-grants-1995_05