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2-Amino-4,6-dichloropyrimidine → N-[4-(2-amino-6-chloropyrimidin-4-ylsulfamoyl)phenyl]-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| 反応物 | N-(4-sulfamoyl-phenyl)-acetamide potassium salt | HCID 70262342 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | N-[4-(2-amino-6-chloropyrimidin-4-ylsulfamoyl)phenyl]-acetamide | HCID 10736032 | 67% |
反応手順
0.98 g (0.006 mol) of 2-amino-4,6-dichloropyrimidine and 3.03 g (0.012 mol) of N-(4-sulfamoyl-phenyl)-acetamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone at 140° C. for 8 hours. Then, the solvent was distilled off in a high vacuum, the residue was partitioned in ethyl acetate/water, the inorganic phase was saturated with sodium chloride and the remaining ethyl acetate dissolved in the aqueous was distilled off on a rotary evaporator. The aqueous phase was made acid with 1N HCl, the crystals which separated were filtered off under section and washed with water. After drying there were obtained 1.37 g (67%) of N-[4-(2-amino-6-chloro-pyrimidin-4-ylsulfamoyl)-phenyl]-acetamide as beige crystals; m.p.: 272-273° C. (dec.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05939451 |
| 出典データセット | uspto-grants-1999_08 |
| ORD ID | ord-448f64558e564d9bb2b60e015117fc2a |
| 出典メモ | uspto-grants-1999_08 |