反応 #558625

ord-bb09df4db3c347ce857da955ffe58b1a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄then washed with 1M aqueous hydrochloric acid
  2. 2
    その他dried
  3. 3
    その他the solvent removed under vacuum
  4. 4
    その他The residue is purified by flash chromatography (0-30% ethyl acetate in cyclohexane)

実験手順

3-Methyl-1,3-butanediol (1.5 mL, 14.06 mmol) is suspended in dry dichloromethane (5 mL) and pyridine (1.24 mL, 15.46 mmol) is added followed by 4-toluenesulfonyl chloride (2.68 g, 14.06 mmol). The mixture is stirred overnight then washed with 1M aqueous hydrochloric acid, dried and the solvent removed under vacuum. The residue is purified by flash chromatography (0-30% ethyl acetate in cyclohexane) to give the title compound. (Yield 970 mg).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08633182B2uspto-grants-2014_01