참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Hydrazine Sulfate | HCID 24842 | — |
| 반응물 | 3-Bromo-4-nitrophthalide | HCID 17985038 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Nitrophthalazin-1(2H)-one | HCID 20323190 | 43.8% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08097627B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_01 |
|---|
| ORD ID | ord-06aba8d2e12342b796ed1d107bd5b231 |
|---|
| 출처 메모 | uspto-grants-2012_01 |
|---|
