Реакция #2331745

ord-ff74a98299234235868ddfca7f0c71d6

Реагенты

Нет

Растворители

Условия реакции

Температура
112.5°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураReflux
  2. 2
    Температураwas maintained for 8-10 hrs
  3. 3
    Другоеwas removed under reduced pressure and 3.5 L of water
  4. 4
    workup.ADDITIONwas added to the concentrated mass
  5. 5
    Другоеat 20° C
  6. 6
    ТемператураThe reaction mass was further cooled to 10° C.
  7. 7
    Другоеto obtain solid
  8. 8
    ФильтрацияThe solid was filtered
  9. 9
    Промывкаwashed with water
  10. 10
    Другоеdried

Методика

3-Amino-4-isobutyl amino quinoline (215 gm, 1.0 mole) was dissolved in formic acid (1000 ml) and further refluxed the reaction mass to 110-115° C. Reflux was maintained for 8-10 hrs. After completion of reaction excess formic acid was removed under reduced pressure and 3.5 L of water was added to the concentrated mass. This diluted mass was then basified with 30% NaOH to pH (10 to 11) at 20° C. The reaction mass was further cooled to 10° C. and stirred for further 3 hrs to obtain solid. The solid was filtered, washed with water and dried to get the title compound (221 gm, 98%) as a white solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07678912B2uspto-grants-2010_03