반응 #306338

ord-07d57b1329624653ab2c2de8abb276a4

용매

반응 조건

온도
-78°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGStirring
  2. 2
    workup.WAITwas continued at −78° C. for 45 min
  3. 3
    기타The reaction mixture was quenched with a satured aqueous solution of NaHCO3
  4. 4
    추출The aqueous layer was extracted with Et2O
  5. 5
    건조The organic extracts were dried over MgSO4
  6. 6
    여과filtered
  7. 7
    농축concentrated in vacuo
  8. 8
    기타Used in the next step without purification (obtained 1.29 g)

실험 절차

Butyllithium (1.6M in THF, 3.5 ml, 5.5 mmol) was added to a stirred solution of 2-methylthiazole (0.45 ml, 5.0 mmol) in THF (15 mL) at −78° C. The reaction mixture was stirred at −78° C. for 40 min. Chlorotrimethylstannane (1M in THF, 5.0 ml, 5.0 mmol) was added. Stirring was continued at −78° C. for 45 min. The reaction mixture was quenched with a satured aqueous solution of NaHCO3. The aqueous layer was extracted with Et2O. The organic extracts were dried over MgSO4, filtered and concentrated in vacuo. Used in the next step without purification (obtained 1.29 g). MS m/z=264.1. Calc'd for C7H13NSSn: 261.94.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08198448B2uspto-grants-2012_06