反応 #1178

ord-7bfae8fa5eb84c9b9f50ce2960b99ca7

反応方程式

O=N[O-].[Na+]
NaNO2
[Cl][Sn][Cl]
SnCl2
Nc1ccc(C(=O)O)c2c1CCCC2
4-amino-5,6,7,8-tetrahydro-1-naphthalenecarboxylic acid
Cl.NNc1ccc(C(=O)O)c2c1CCCC2
hydrazine
収率 73.3%
Cl.NNc1ccc(C(=O)O)c2c1CCCC2
4-Hydrazino-5,6,7,8-tetrahydro-1-naphthalene-carboxylic acid hydrochloride
収率 73.3%

反応条件

温度
-5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe mixture is stirred for 1 hour at RT
  2. 2
    ろ過filtered
  3. 3
    洗浄the product is washed with concentrated HCl
  4. 4
    その他dried under a stream of dry nitrogen

実験手順

A solution of 0.26 g of NaNO2 in 1 ml of water is added to a solution, cooled to -5° C., of 0.73 g of 4-amino-5,6,7,8-tetrahydro-1-naphthalenecarboxylic acid in 10 ml of concentrated HCl. After one and a half hours of stirring at -5° C., a solution of 3.4 g of SnCl2 ·2H2O in 34 ml of concentrated HCl is added at -5° C. The mixture is stirred for 1 hour at RT and filtered, and the product is washed with concentrated HCl and dried under a stream of dry nitrogen to obtain 0.67 g of the expected hydrazine.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723483uspto-grants-1998_03