تفاعل #1180

ord-b8001a84916e479bb360b2e627d79199

معادلة التفاعل

[Cl][Sn][Cl]
SnCl2
O=N[O-].[Na+]
NaNO2
COc1cc(C(=O)O)ccc1N
4-amino-3-methoxybenzoic acid
COc1cc(C(=O)O)ccc1NN.Cl
4-Hydrazino-3-methoxybenzoic acid hydrochloride

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture is cooled to -10° C.
  2. 2
    workup.STIRRINGAfter one and a half hours of stirring at -10° C.
  3. 3
    ترشيحthe mixture is filtered
  4. 4
    غسيلthe precipitate is washed with 50 ml of pentane
  5. 5
    أخرىto obtain
  6. 6
    أخرىafter drying

الإجراء التجريبي

A solution of 2.17 g of NaNO2 in 40 ml of H2O is added slowly to a solution, cooled to 0° C., of 5 g of 4-amino-3-methoxybenzoic acid in 50 ml of concentrated HCl. After 1 hour 15 minutes of stirring at 0° C., the mixture is cooled to -10° C., and a solution of 23.6 g of SnCl2 ·2H2O in 20 ml of concentrated HCl and 20 ml of water is added over 30 min. After one and a half hours of stirring at -10° C., the mixture is filtered, and the precipitate is washed with 50 ml of pentane to obtain, after drying, 6 g of expected product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05723483uspto-grants-1998_03