Реакция #4479

ord-f29eda88a35249c99e36ce3a1f68295a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеat ca. 0°
  2. 2
    Другоеthe temperature below 0° C
  3. 3
    workup.STIRRINGThe suspension was stirred for a further 30 min
  4. 4
    Фильтрацияfiltered
  5. 5
    Промывкаwashed with dried ether

Методика

A suspension of 3-methoxyaniline (10 g) in concentrated hydrochloric acid (85 ml) was stirred at ca. 0° and a solution of sodium nitrite (5.75 g) in water (25 ml) was slowly added over a period of 30 min keeping the temperature of the mixture at ca. 0°. After 1 h a solution of tin II chloride dihydrate (59 g) in concentrated hydrochloric acid (50 ml) was added over a period of 1.5 h, to the cooled suspension keeping the temperature below 0° C. The suspension was stirred for a further 30 min, filtered and washed with dried ether to give the title compound as a solid (14 g) m.p. 171°.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04725615uspto-grants-1988_02