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Dimethylformamide → HCID 14116990、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Amino-3-chloropyrazine | HCID 276224 | — |
| 反応物 | HCID 13578027 | HCID 13578027 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | HCID 14116990 | HCID 14116990 | — |
反応手順
Following the general procedure of Example 5(B), 3.88 g. of 2-amino-3-chloropyrazine and 9.21 g. of α-bromo-2-methoxy-4-methylsulfonylacetophenone were reacted to give 4.8 g. of the intermediate 8-chloro-2-(2-methoxy-4-methylsulfonylphenyl)imidazo[1,2-a]pyrazine hydrobromide. The hydrobromide salt (3.6 g.) was hydrogenated in 195 ml. of dimethylformamide and 2.7 g. of triethylamine in the presence of 1 g. of 5% palladium-on-barium sulfate. After filtration, the solution was poured into 700 ml. of ethyl acetate, washed four times with a saturated sodium chloride solution and the solvent concentrated in vacuo. At a reduced volume crystallization occurred and 540 mg. of the title product were recovered by filtration.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04537889 |
| 出典データセット | uspto-grants-1985_08 |
| ORD ID | ord-29317c573c724011aff33092497ceb2c |
| 出典メモ | uspto-grants-1985_08 |