Реакция #302891

ord-a6b385fe4dc24e14bfda5cf07e02255c

Уравнение реакции

Cl.Clc1cccc(CNC2=NCCS2)c1Cl
((2,3-dichlorophenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride
Cl.Clc1cccc(CNC2=NCCS2)c1Cl
Compound C7
Cl.Clc1cccc(CNC2=NCCS2)c1Cl
((2,3-dichlorophenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride
[Na+].[OH-]
sodium hydroxide
Clc1cccc(CNC2=NCCS2)c1Cl
title compound
Выход 98.9%
Clc1cccc(CNC2=NCCS2)c1Cl
((2,3-dichlorophenyl)methyl)-1,3-thiazolin-2-ylamine
Выход 98.9%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONpoured into a separatory funnel
  2. 2
    Экстракцияwas extracted with two 50 mL portions of diethyl ether
  3. 3
    Сушкаdried with sodium sulfite
  4. 4
    Фильтрацияfiltered
  5. 5
    КонцентрированиеThe filtrate was concentrated under reduced pressure

Методика

A mixture of 0.36 gram (0.0012 mole) of ((2,3-dichlorophenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride (Compound C7) in one mL of water was added to a stirred, cold (ice water bath) mixture of 0.05 gram (0.0013 mole) of sodium hydroxide in 10 mL of water and 10 mL of diethyl ether. The reaction mixture was stirred for 10 minutes, poured into a separatory funnel and was extracted with two 50 mL portions of diethyl ether. The extracts were combined, dried with sodium sulfite and filtered. The filtrate was concentrated under reduced pressure to yield 0.31 gram of the title compound as a white solid. The NMR spectrum was consistent with the proposed structure.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08193118B2uspto-grants-2012_06