반응 #58555

ord-5e62bed0301d4377be51ee6ea4eb4aca

반응 조건

온도
22°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과Next, the reaction mixture was filtered
  2. 2
    농축concentrated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in anhydrous MeOH (25 ml)
  4. 4
    농축The MeOH was concentrated
  5. 5
    기타triturated with ether producing

실험 절차

The product from step f) (409 mg, 1.52 mmol) in dichloroethane (8 ml) was treated with K2CO3 (839 mg, 6.08 mmol) and Ace-Cl (658 μl, 6.08 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 hour at 22° C. The MeOH was concentrated and triturated with ether producing to give 215 mg (66%) of the subtitle compound as its HCl salt. MS calculated for C10H13NS+H 180, observed 180.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07423056B2uspto-grants-2008_09