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Ethyl 2-methoxyacetate → Ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 2-methoxyacetate | HCID 77544 | — |
| 反応物 | 4-Amino-3-cyano-6-fluoro-5-hydroxy-2-methylbiphenyl | HCID 86097446 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Ethyl 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxylate | HCID 51041426 | 96% |
反応手順
4-Amino-6-fluoro-5-hydroxy-2-methylbiphenyl-3-carbonitrile (I-41) (5.0 g, 20.64 mmol) and ethyl methoxyacetate (18.18 g, 82.56 mmol) were stirred at 100° C. for 23 hours under nitrogen atmosphere. The reaction liquid was cooled to room temperature, and left at the same temperature for 17 hours. At 0° C., hexane was added to the suspension, and left at the same temperature for 1 hour. With washing with hexane, the precipitated crystal was collected by filtration. The crystal was collected, dried at 50° C. under reduced pressure for 4 hours, and then at room temperature for 12 hours to obtain the entitled compound (6.39 g, 96%) as a pale brown powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737166B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-59785a76fe4444ebbfba8c01f827d571 |
| 出典メモ | uspto-grants-2010_06 |