Potassium Carbonate → 4,5,6,7,7a,8-Hexahydro-3bH-1-thia-5-aza-cyclopenta[alpha]indene

Temperatur

22 °C

The product from step g) (963 mg, 3.58 mmol) in dichloroethane (18 ml) was treated with K2CO3 (1.97 g, 14.3 mmol) and Ace-Cl (1.54 ml, 14.3 mmol) at 80° C. for 16 hours. Next, the reaction mixture was filtered, concentrated and the residue was dissolved in anhydrous MeOH (25 ml) and stirred for 1 h at 22° C. The MeOH was concentrated and triturated with ether to give 467 mg (61%) of the subtitle compound. MS calculated for C10H13NS+H 180, observed 180.

1. filtrationNext, the reaction mixture was filtered
2. concentrationconcentrated
3. dissolutionthe residue was dissolved in anhydrous MeOH (25 ml)
4. concentrationThe MeOH was concentrated
5. customtriturated with ether

ORD-Eintrag

ord-ef4fca7745fa46aa8999547abfab36bb

Quelldatensatz

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07423056B2