Reaktion #1667152

Reaktionsgleichung

2-mercaptoethanol

7-chloro-2,3-dihydro-5-phenyl-1H-1,4-benzodiazepine

7-chloro-5-phenyl-3H-1,4-benzodiazepine

acetic acid

→

product

7-chloro-2,3-dihydro-2-(2-hydroxyethylthio)-5-phenyl-1H-1,4-benzodiazepine

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturunder reflux overnight
3. 3
   EinengenThe resulting solution was concentrated under reduced pressure until the product
4. 4
   Sonstigeto crystallize
5. 5
   workup.ADDITIONdiluted with 100 ml of ether
6. 6
   SonstigeThe product was collected
7. 7
   Waschenwashed with ether

Vorschrift

7-chloro-2,3-dihydro-5-phenyl-1H-1,4-benzodiazepine (10 g) was oxidized to 7-chloro-5-phenyl-3H-1,4-benzodiazepine as described in Example 1 with the addition of 0.1 ml of acetic acid. The crude oxidation product was taken up in THF (60 ml), treated with 2-mercaptoethanol (10 ml ) and heated under reflux overnight. The resulting solution was concentrated under reduced pressure until the product began to crystallize and then diluted with 100 ml of ether. The product was collected and washed with ether to give the above-named product as colorless crystals, mp 135°-140° (dec).

Quelle