반응 #1516733

ord-65df8d71905e489c8c33bfbb665a836f

용매

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도It was cooled to rt
  2. 2
    기타The solid was collected
  3. 3
    여과via filtering
  4. 4
    workup.DISSOLUTIONThe solid was dissolved in hot EtOH (0.5 mL)
  5. 5
    기타the vial was sealed
  6. 6
    온도slowly cooled to rt
  7. 7
    기타The precipitate was collected
  8. 8
    여과via filtering

실험 절차

A suspension of 6-(1-(5-bromopentylsulfonyl)-1,2,3,6-tetrahydropyridin-4-yl)-2-(1-(5-propylpyrimidin-2-yl)piperidin-4-yloxy)benzo[d]thiazole (Example 30C, 22.8 mg, 0.035 mmol) in EtOH (1.5 mL) and Et3N (0.75 mL) was heated in microwave at 120° C. for 40 min. It was cooled to rt, Et2O (2 mL) was added. The solid was collected via filtering. The solid was dissolved in hot EtOH (0.5 mL), the vial was sealed and slowly cooled to rt. The precipitate was collected via filtering to afford the desired product as a white solid (15 mg, 51% yield). LCMS (m/z)=669 (M+H)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08940716B2uspto-grants-2015_01