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10th December 2016 @ 04:57
New: New

Date of Reaction: 11/23

CC1=NC(C)=C(N=C1Cl)Cl

 

Procedure:

Excess phosphoryl chloride (5.0mL, 0.0535 mol) was added to the oxidized dimethyl product (1.2g, 0.008 mol). The mixture was stirred and refluxed for 1.5 hours at 70oC. The reaction mixture was then alkalized using 20% NaOH. An extraction was carried out with CHCl3 (3 x 20 mL). Next steps will be to run a column chromatography on that product and then to get NMR data.

 

Table of Reagents (Rxn2) DiMethyl

 
 
 
 
 

Reagent

mass (g)

mols

Molecular Weight (g/mol)

Volume (mL)

Density (g/mL)

Product RxN1

1.200

0.008

158.590

 
 

Phosphoryl Chloride

3.481

0.023

153.333

2.122

1.640

Product RxN2 Dimethyl

1.347

0.008

178.040

 
 
 
 
 
 

*Used 5 mL of POCl3

 

Attached are TLCs 

Attached Files
Second Step Synthesis of 6:8.pdf