تفاعل #1183

ord-e46e69b904a7491db50b6afa5f24b6f5

معادلة التفاعل

O=N[O-].[Na+]
NaNO2
[Cl][Sn][Cl]
SnCl2
Cc1ccc(C(=O)O)cc1N
3-amino-4-methylbenzoic acid
Cc1ccc(C(=O)O)cc1NN.Cl
3-Hydrazino-4-methylbenzoic acid hydrochloride

الكواشف

لا شيء

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    workup.WAITthe mixture is left
  2. 2
    درجة الحرارةAfter cooling to -10° C.
  3. 3
    workup.STIRRINGAfter stirring for 1 hour at RT
  4. 4
    ترشيحfiltration
  5. 5
    غسيلwashing of the precipitate with 5 ml of 1N HCl
  6. 6
    تجفيفdrying over P2O5 under vacuum, 6.15 g of the expected product
  7. 7
    أخرىare obtained

الإجراء التجريبي

A solution of 2.74 g of NaNO2 in 28 ml of water is added over 30 minutes to a solution, cooled to -5° C., of 5 g of 3-amino-4-methylbenzoic acid in 120 ml of concentrated HCl and 40 ml AcOH, and the mixture is left stirring for 1 hour 20 minutes at 0° C. After cooling to -10° C., a solution of 27.6 g of SnCl2 ·2H2O in 28 ml of concentrated HCl is added slowly. After stirring for 1 hour at RT, filtration, washing of the precipitate with 5 ml of 1N HCl and drying over P2O5 under vacuum, 6.15 g of the expected product are obtained.

المصدر

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