反应 #69629

ord-4b7498d6d4404f80b161caa37cf7fac8

溶剂

反应条件

温度
25°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with water
  2. 2
    其他After removing the aqueous layer the organic layer
  3. 3
    其他is azeotropically dried
  4. 4
    浓缩concentrated

实验过程

To form 2,3-dichloro-6-nitrobenzylalcohol (compound XX) from 2,3-dichloro-6-nitro benzaldehyde (compound XIX), compound XIX is preferably solubilized in a solvent or solvent mixture such as toluene and methanol. The solution of compound XIX is added to a reducing solution such as sodium borohydride in an organic solvent over a period of time to maintain a reaction temperature below about 40° C., preferably 25° C. The reaction is preferably stirred for 24 hours at room temperature under nitrogen and then washed with water. After removing the aqueous layer the organic layer is azeotropically dried and concentrated forming 2,3-dichloro-6-nitrobenzylalcohol (compound XX).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08530651B2uspto-grants-2013_09