Reaktion #302891

ord-a6b385fe4dc24e14bfda5cf07e02255c

Reaktionsgleichung

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
Ausbeute 98.9%
Clc1cccc(CNC2=NCCS2)c1Cl
((2,3-dichlorophenyl)methyl)-1,3-thiazolin-2-ylamine
Ausbeute 98.9%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONpoured into a separatory funnel
  2. 2
    Extraktionwas extracted with two 50 mL portions of diethyl ether
  3. 3
    Trocknendried with sodium sulfite
  4. 4
    Filtrationfiltered
  5. 5
    EinengenThe filtrate was concentrated under reduced pressure

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08193118B2uspto-grants-2012_06