Реакция #530742

ord-c6ba4a1021be4a4b8948473fc61a6e5b

Уравнение реакции

ClCCl
methylene chloride
O=C(Cc1cccc(Cl)n1)N(F)N(F)F
2-chloro-6-hydrazinopyridine
O=C(Cc1cccc(Cl)n1)N(F)N(F)F
2-(6-Chloro-2-pyridyl)trifluoroacetic acid, hydrazide
c1ccncc1
pyridine
ClCCl
methylene chloride
CC(Br)C(=O)Cl
2-bromopropionyl chloride
CC(Br)(C(=O)NN)c1cccc(Cl)n1
2-(6-Chloro-2-pyridyl)-2-bromopropionic acid, hydrazide

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONA mixture of 2.1 g
  2. 2
    workup.ADDITIONis treated with 2.75 g
  3. 3
    ДругоеAfter a heavy precipitate forms the ice bath is removed
  4. 4
    ДругоеThe precipitate is collected
  5. 5
    Промывкаwashed with methylene chloride
  6. 6
    Другоеto provide 2.6 g

Методика

A mixture of 2.1 g. of 2-chloro-6-hydrazinopyridine (prepared in Example 1), 1.25 g. of pyridine and 50 ml. of methylene chloride is cooled to 10° C. and is treated with 2.75 g. of 2-bromopropionyl chloride in 5 ml. of methylene chloride according to the procedure of Example 2. After a heavy precipitate forms the ice bath is removed and the reaction mixture is stirred at room temperature for 1/2 hour. The precipitate is collected and washed with methylene chloride to provide 2.6 g. of the product of the Example as a colorless solid m.p. 184° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04260767uspto-grants-1981_04