反応 #165701

ord-7a7fd07a31984e249677bcd4f6de1b19

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the mixture was extracted with ethyl acetate (2×50 mL)
  2. 2
    洗浄The combined organics were washed with H2O (2×50 mL)
  3. 3
    乾燥dried over MgSO4
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated under reduced pressure
  6. 6
    その他dried under vacuum (˜1 mm Hg)

実験手順

To a solution of 3-methylbutane-1,3-diol (2.13 mL, 20 mmol) in pyridine (20 mL) at 0° C. was added para-toluenesulfonyl chloride (3.8 g, 20 mmol) in pyridine (10 mL) drop-wise over 15 minutes. This mixture stirred at ambient temperature for 3 hours and 35 mL H2O was added and the mixture was extracted with ethyl acetate (2×50 mL). The combined organics were washed with H2O (2×50 mL), dried over MgSO4, filtered, concentrated under reduced pressure and dried under vacuum (˜1 mm Hg) to afford the title compound. MS (ESI) m/z 276 (M+18)+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08841334B2uspto-grants-2014_09