反应 #71532

ord-2ae19a871ca64856a3312bef045f65b0

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooled to 0° C
  2. 2
    workup.STIRRINGthe reaction mixture was stirred for 2 h
  3. 3
    温度cooled to 0° C
  4. 4
    洗涤The organic layer was washed with brine in water (1:1, 2×1 L)
  5. 5
    workup.ADDITIONMeTHF (1 L) was added

实验过程

To a mixture of 2,2-diethoxyethylamine (209 mL, 1.43 mol) and MeTHF (1050 L) was added cyclohexanecarbaldehyde (107 mL, 0.89 mol). The reaction mixture was stirred for 30 min at room temperature and cooled to 0° C. Sodium triacetoxyborohydride (378 g, 1.79 mol) was added over 40 min and the reaction mixture was stirred for 2 h and cooled to 0° C. 1 M NaOH (1 L) was added. The organic layer was washed with brine in water (1:1, 2×1 L) and the volume was reduced to ˜20%. MeTHF (1 L) was added and the volume reduced to ˜20%. The solution of the crude title intermediate was used directly in the next step.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08536335B2uspto-grants-2013_09