تفاعل #10476

ord-46a2b70cb3774dc384354d92898d7d21

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلapprox. 70 ml of water and washed three times with in each case approx. 50 ml of n-heptane
  2. 2
    استخلاصare extracted with 50 ml of 1:1 methanol/water
  3. 3
    غسيلThe combined aqueous phases are washed again with n-heptane
  4. 4
    تركيزAfter concentrating the aqueous phase

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07094795B2uspto-grants-2006_08