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With triethylamine; In N-methyl-acetamide; water; ethyl acetate;
b. Diethyl (4,6-dichloro-m-phenylene)dioxamate To a solution of 31.9 gm. (0.18 mole) of 1,3-diamino-4,6-dichlorobenzene in 75 ml. of dry dimethylformamide is added 300 ml. of dry ethyl acetate and 43.6 gm. (0.432 mole) of triethylamine. The resulting solution is cooled to 0 in an ice-bath. To the stirred solution is added dropwise 59.0 gm. (0.432 mole) of ethyl oxalyl chloride, keeping the temperature below 15. The mixture is stirred in the ice-bath for 1 hour and then allowed to stand at room temperature for 48 hours. Most of the solvents are removed by distillation under reduced pressure. The residue is poured into 1 liter of cold water. The precipitate is removed by filtration and recrystallized from ethanol. There is obtained 55.3 gm. (81%) of long colorless needles melting at 124-5. Analysis Calc'd. for: C14 H14 Cl2 N2 O6 C, 44.58; H, 3.74; Cl, 18.80; N, 7.43. Found: C, 44.67; H, 3.75; Cl, 18.90; N, 7.74.
Preparation of B-5a:A solution of 2,4-dichloro-5-amino-aniline (4.1 g, 23.2 mmol) in DMF (50 mL) is combined with potassium-ethylxanthogenate and stirred for 3 days at 150 0C. After cooling to RT the mixture is diluted with ice water and acidified with aqueous HCl. The precipitate is filtered off and dried in vacuo until a constant weight is obtained. The title compound is used in the next reaction without further purification (HPLC tRet = 3.9 min; MS [M+H]+: m/z = 261).
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