참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | 5-Chloro-1-indanone | HCID 142599 | — |
| 반응물 | Diaminomaleonitrile | HCID 2723951 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | HCID 16065919 | HCID 16065919 | — |
반응 단계
A mixture of 5-chloro-1-indanone (1.05 g, 6.28 mmol) and N-bromosuccinimide (2.23 g, 12.56 mmol) in DMSO (25 ml) was stirred overnight at 40° C. and 5 h at 80° C. under vacuum. Water (125 ml) was added and the mixture was extracted with CH2Cl2 (25 ml). The aqueous phase was saturated with brine and solid NaCl and extracted with CH2Cl2 (4×80 ml). The collected organic phases were dried over Na2SO4 and the solvent evaporated. The crude was dissolved in EtOH (63 ml), diaminomaleonitrile (678 mg, 6.28 mmol) and a catalytic amount of AcOH were added and the mixture stirred at 80° C. for 45 min. The precipitate was collected by filtration and washed with EtOH (464 mg). The filtered solution was evaporated and the crude purified by flash.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08648076B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_02 |
|---|
| ORD ID | ord-277339e11b364d9fb2cd6bac8bd778bc |
|---|
| 출처 메모 | uspto-grants-2014_02 |
|---|