반응 #1182

ord-b9463e90fa6b413699ae9fcde2e663de

반응 방정식

[Cl][Sn][Cl]
SnCl2
O=N[O-].[Na+]
NaNO2
Nc1ccc(Cl)c(C(=O)O)c1
5-amino-2-chlorobenzoic acid
Cl.NNc1ccc(Cl)c(C(=O)O)c1
expected product
수율 123.1%
Cl.NNc1ccc(Cl)c(C(=O)O)c1
5-Hydrazino-2-chlorobenzoic acid hydrochloride
수율 123.1%

반응 조건

온도
-3°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to -10° C.
  2. 2
    workup.STIRRINGThe mixture is stirred for one and a half hours at 0° C.
  3. 3
    여과filtered
  4. 4
    기타the precipitate is dried

실험 절차

A solution of 2.11 g of NaNO2 in 40 ml of water is added over 30 minutes to a suspension, cooled to -2° C., of 5 g of 5-amino-2-chlorobenzoic acid in 50 ml of concentrated HCl. The solution is stirred for 2 hours at -3° C. and cooled to -10° C., and a solution of 23 g of SnCl2 ·2H2O in 20 ml of concentrated HCl and 20 ml of water is added over 30 minutes. The mixture is stirred for one and a half hours at 0° C. and filtered, and the precipitate is dried to obtain 4 g of expected product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723483uspto-grants-1998_03