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CAS No. : | 74587-12-5 | MDL No. : | MFCD06656566 |
Formula : | C7H8INO | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | UHPNLGCUIGEZRB-UHFFFAOYSA-N |
M.W : | 249.05 | Pubchem ID : | 22054596 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | In isopropyl alcohol;Heating / reflux; | EXAMPLE 20 2-Cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-[(3-iodo-4-methoxyphenyl)amino]prop-2-enamide To a suspension of <strong>[846023-24-3]2-cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide</strong> (5.00 g, 19.30 mol) in 400 mL of iso-propanol, under N2, was added 3-iodo-p-anisidine (5.80 g, 23.16 mmol). This mixture was heated to reflux to give a clear yellow solution. To this solution, triethylorthoformate (8.60 mL, 52.11 mmol) was added dropwise and the reaction mixture was heated at reflux overnight. An additional 10 mL of triethylorthoformate was added and the mixture was heated at reflux overnight. The mixture was allowed to cool to room temperature and the white solid was collected by filtration, washed with isopropanol, and dried overnight at ~40 C. under reduced pressure. Purification by suspension in hot ethyl acetate followed by addition of cold hexanes gave 8.50 g (85%) of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-[(3-iodo-4-methoxyphenyl)amino]prop-2-enamide as a yellow solid, mp 289-290 C.; MS (ES) m/z 516.7 (M-H)- Analysis for C18H14Cl2IN3O3; Calcd: C, 41.73; H, 2.72; N, 8.11. Found: C, 40.66; H, 2.94; N, 7.90. |
85% | In isopropyl alcohol;Heating / reflux; | Reference Example 2; 2-Cyano-N-(2,4-dichloro-5-methoxyphenyl )-3-r(3-iodo-4-methoxyphenv?amino1- prop-2-enamide; To a suspension of <strong>[846023-24-3]2-cyano-N-(2,4-dichloro-5-methoxyphenyl)acetamide</strong> (5.00 g, 19.30 mol) in 400 ml_ of /so-propanol, under N2, is added 3-iodo-p-anisidine (5.80 g, 23.16 mmol). This mixture is heated to reflux to give a clear yellow solution. To this solution, triethylorthoformate (8.60 ml_, 52.11 mmol) is added dropwise and the reaction mixture is heated at reflux overnight. An additional 10 ml_ of triethylorthoformate is added and the mixture is heated at reflux overnight. The mixture is allowed to cool to room temperature and the white solid is collected by filtration, washing with /so-propanol, and dried overnight at -4O0C under reduced pressure. Purification by suspension in hot ethyl acetate followed by addition of cold hexanes gives 8.50 g (85%) of 2-cyano-N-(2,4-dichloro-5-methoxyphenyl)-3-[(3-iodo- 4-methoxyphenyl)amino]prop-2-enamide as a yellow solid, mp 289-290 0C; MS (ES) m/z 516.7 (M-H)-. Analysis for C18H14CI2IN3O3:Calcd: C, 41.73; H, 2.72; N, 8.11. Found: C, 40.88; H, 2.64; N, 7.90. |
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