반응 #9768

ord-bb369774dd52483faa7fe8c2c2fb6a6b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    추출The mixture was extracted with water, 2M aqueous sodium hydroxide, water
  3. 3
    건조dried with brine and over sodium sulfate
  4. 4
    기타The crude product was purified by Biotage chromatography®

실험 절차

A solution of (3-methylthien-2-yl)methanol (3.20 g) in tetrahydrofuran (10 ml) was added to a mixture of sodium hydride (60% dispersion in mineral oil, 1.05 g) in tetrahydrofuran (40 ml). After the evolution of hydrogen had subsided triisopropylsilyl chloride (5.2 ml) was added. The reaction mixture was stirred for 2 hours then diluted with ethyl acetate. The mixture was extracted with water, 2M aqueous sodium hydroxide, water and dried with brine and over sodium sulfate. The crude product was purified by Biotage chromatography® using 100:1 petroleum ether:ethyl acetate as eluent to give the title compound as a colorless oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091237B2uspto-grants-2006_08