関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (2S)-2-(2,3,4-Trifluoroanilino)propanol | HCID 11401466 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (3S)-3-Methyl-7,8-difluoro-2,3-dihydro-4H-1,4-benzoxazine | HCID 11041424 | 66.5% |
反応手順
To DMF (2 ml) was added sodium hydride (39 mg) and the mixture was heated to 60° C. in an oil bath. Next, a solution of the compound (100 mg) obtained in Example 51 in DMF was dropped there into and the obtained mixture was stirred for 1 hour. After treating in a conventional manner, the mixture was subjected to silica gel column chromatography to give 60 mg (66%) of the title compound. The optical purity determined by HPCL was >94% ee. Various spectral data was identical with those of a specimen synthesized separately.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07189847B2 |
|---|
| 出典データセット | uspto-grants-2007_03 |
|---|
| ORD ID | ord-0faf5520239f44f386be0d5f67aff3e1 |
|---|
| 出典メモ | uspto-grants-2007_03 |
|---|
