Reaktion #322855

Reaktionsgleichung

( 2 )

(2RS)-2-cyclopentyl-2-methyl-5-acetylthio-6,7-dichloroindan-1-one

methanol

sodium hydroxide

→

title compound

(2RS)-2-cyclopentyl-2-methyl-5-mercapto-6,7-dichloroindan-1-one

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthen concentrated under reduced pressure
2. 2
   workup.ADDITION2 ml of water was added to the residue
3. 3
   Temperaturunder cooled with ice
4. 4
   ExtraktionThe mixture was extracted with diethyl ether
5. 5
   Waschenthe extract was washed successively with water
6. 6
   Trocknena saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate
7. 7
   Einengenconcentrated under reduced pressure

Vorschrift

To a solution of 300 mg of 5-acetylthio compound prepared in (2) in the mixture of 1.3 ml of methanol and 0.6 ml of tetrahydrofuran was dropped 1.35 ml of 5% aqueous solution of sodium hydroxide and the mixture was stirred for 20 minutes at ambient and then concentrated under reduced pressure. 2 ml of water was added to the residue and the mixture was acidified to pH 1 with 1N hydrochloric acid under cooled with ice. The mixture was extracted with diethyl ether and the extract was washed successively with water and a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to give 210 mg of the title compound as crude product having following physical data.

Quelle