反应 #1375803

ord-61808bd61e0c4951bd74b0eb2dc32d2e

反应方程式

Cl.Cn1nnc2ccc(C(NN)c3ccc(Cl)cc3)cc21
intermediate 2-b
Cl.Cn1nnc2ccc(C(NN)c3ccc(Cl)cc3)cc21
(-)-6-[(4-chlorophenyl)-hydrazinomethyl]-1-methyl-1H-benzotriazole monohydrochloride
[Na+].[OH-]
sodium hydroxide
Cn1nnc2ccc(CNNc3ccc(Cl)cc3)cc21
(-)-6-[(4-chlorophenyl)hydrazinomethyl]-1-methyl-1H-benzotriazole

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the organic layer was separated
  2. 2
    其他evaporated
  3. 3
    温度The residue and 1.4 g of potassium hydroxide were refluxed in 50 ml ethanol for 3 hours

实验过程

To a suspension of 8.1 g of intermediate 2-b in 60 ml of dichloromethane was added a solution of 1 g sodium hydroxide in 15 ml of water. The whole was stirred for 15 min., then the organic layer was separated and evaporated. The residue and 1.4 g of potassium hydroxide were refluxed in 50 ml ethanol for 3 hours, yielding (-)-6-[(4-chlorophenyl)hydrazinomethyl]-1-methyl-1H-benzotriazole (interm. 2-c); enantiomeric excess: 20%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05746840uspto-grants-1998_05