関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Hydrazine Sulfate | HCID 24842 | — |
| 反応物 | 3-Bromo-4-nitrophthalide | HCID 17985038 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Nitrophthalazin-1(2H)-one | HCID 20323190 | 43.8% |
反応手順
18.25 g of hydrazine sulfate and 14.88 g of sodium carbonate are stirred in 300 ml of DMF at 100° C. for one hour. Then, 7.24 g of 3-bromo-4-nitro-phthalide in 100 ml of DMF is added, and it is stirred for another 4 hours at 100° C. It is added to water, extracted several times with ethyl acetate, and the organic phase is washed with water and brine. It is dried, and the solvent is removed in a vacuum. After recrystallization from ethyl acetate, 2.35 g of 5-nitro-phthalazin-1-one is obtained as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08097627B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-06aba8d2e12342b796ed1d107bd5b231 |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|
