反応 #10476

ord-46a2b70cb3774dc384354d92898d7d21

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄approx. 70 ml of water and washed three times with in each case approx. 50 ml of n-heptane
  2. 2
    抽出are extracted with 50 ml of 1:1 methanol/water
  3. 3
    洗浄The combined aqueous phases are washed again with n-heptane
  4. 4
    濃縮After concentrating the aqueous phase

実験手順

10 g of the crude acetate/alcohol mixture from Example 29 were taken up in approx. 90 ml of methanol and approx. 70 ml of water and washed three times with in each case approx. 50 ml of n-heptane. The combined heptane phases (contain predominantly the acetate) are extracted with 50 ml of 1:1 methanol/water. The combined aqueous phases are washed again with n-heptane. After concentrating the aqueous phase, 3.6 g of the desired (1S,3R)-3-benzyloxycyclohexan-1-ol were obtained, and the concentration of the combined heptane phases gave 5.5 g of the (1R,3S)-acetate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07094795B2uspto-grants-2006_08