化工社化工社 化学情報印刷レポート · 研究参考用
Dimethyl Sulfide → 6-nitro-3,4-dihydro-2H-1,4-benzoxazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfide | HCID 1068 | — |
| 反応物 | 6-Nitro-2H-1,4-benzoxazin-3(4H)-one | HCID 2763683 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-nitro-3,4-dihydro-2H-1,4-benzoxazine | HCID 7062225 | 89.5% |
反応手順
A solution of BH3.Me2S in THF (2 M, 7.75 mL, 15.5 mmol) was added dropwise to a suspension of 6-nitro-4H-benzo[1,4]oxazin-3-one (0.6 g, 3.1 mmol) in THF (10 mL). The mixture was stirred at room temperature overnight. The reaction was quenched with MeOH (5 mL) at 0° C. and then water (20 mL) was added. The mixture was extracted with Et2O and the combined organic layers were washed with brine, dried over Na2SO4 and concentrated to give 6-nitro-3,4-dihydro-2H-benzo[1,4]oxazine as a red solid (0.5 g, 89%), which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741925B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-1dcdfc0ddf624765a8f910386261db07 |
| 出典メモ | uspto-grants-2014_06 |