反应 #71532
ord-2ae19a871ca64856a3312bef045f65b0
反应方程式
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度cooled to 0° C
- 2workup.STIRRINGthe reaction mixture was stirred for 2 h
- 3温度cooled to 0° C
- 4洗涤The organic layer was washed with brine in water (1:1, 2×1 L)
- 5workup.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.