반응 #454041

ord-891cc2ba15b04d7b843f32e705f27aa2

용매

반응 조건

온도
-40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to warm to room temperature
  2. 2
    여과At room temperature the mixture was filtered
  3. 3
    기타dried

실험 절차

n-Butyllithium (77 mL, 192.5 mmol, 2.5 M solution in hexane) was added dropwise at -78° C. to a solution of 3,4-(ethylenedioxy)thiophene (25 g, 175.9 mmol) in anhydrous THF (100 mL) under nitrogen. The solution was stirred for 1 h and warmed to -40° C. Tributylstannyl chloride (85.89 g, 263.9 mmol) was added and the entire solution was finally allowed to warm to room temperature. At room temperature the mixture was filtered using Celite and the solvent was stripped. The organo-tin compound was vacuum dried to give 2-(tributylstannyl)-3,4-(ethylenedioxy)thiophene, obtained as a dark yellow liquid, yield=98%. MS(EI) m/z (rel int): 375 [(M)+ --C4H8, 100%] and 319[(M)+ --C8H16, 18%].

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06130339uspto-grants-2000_10