5-Methoxyacetamido-2,4,6-triiodoisophthaloyl chloride synthesis
- Product Name:5-Methoxyacetamido-2,4,6-triiodoisophthaloyl chloride
- CAS Number:76350-03-3
- Molecular formula:C11H6Cl2I3NO4
- Molecular Weight:667.79
38870-89-2
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Yield:76350-03-3 93%
Reaction Conditions:
in 1,4-dioxane at 80 - 90;
Steps:
2 Example 2[119]Preparation of 5-methoxyacetylamino-2,4,6-triiodoisophthalic acid dichloride (Chemical Formula 1) II
Example 2[119]Preparation of 5-methoxyacetylamino-2,4,6-triiodoisophthalic acid dichloride (Chemical Formula 1) II[120]2.0 kg of 5-amino-2,4,6-triiodoisophthalic acid dichloride and 1.0 L of 1,4-dioxane were added to the first reactor at room temperature (20 to 25), and then 0.95 kg of methoxyacetyl chloride was added thereto. The mixture was stirred at 80 to 90 for 2 to 4 hours to complete the reaction. After completion of the reaction, the reaction solution was cooled to 10 to 15, and then 6 L of ethanol was added thereto. 11.4 L of water was added to the second reactor and the reaction solution was added dropwise and stirred for 30 minutes, followed by filtration. After filtration, the resultant was dried under vacuum at 40 to 60 to obtain the title compound (compound of Chemical Formula 1) in the yield of 93%.[121]1H NMR(DMSO-D6, 500MHz) : 10.18 (s, 1H), 4.03 (s, 2H), 3.47 (s, 3H)
References:
WO2015/60657,2015,A1 Location in patent:Paragraph 118-121
