참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | 1,4-Dichlorophthalazine | HCID 78490 | — |
| 반응물 | 6-(Piperazin-1-yl)pyridine-3-carbonitrile | HCID 2737184 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6-[4-(4-Chloro-phthalazin-1-yl)-piperazin-1-yl]-nicotinonitrile | HCID 44186379 | 51.1% |
반응 단계
To a 100-mL round-bottom flask is added 6-piperazin-1-yl-nicotinonitrile (9.60 g, 50 mmol), 1,4-dichlorophthalazine (11.2 g, 55.1 mmol, 1.1 eq), Et3N (3.5 mL, 250 mmol, 5 eq.), and NMP (100 mL). The mixture is heated to 80° C. for 2.5 h. Upon cooling to room temperature, the reaction is poured into H2O (500 mL) and the precipitate isolated by filtration, rinsing with additional H2O. Crude material is purified by recrystallization (CH2Cl2:heptanes) to afford 8.96 g title compound as a beige solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08536168B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-69b2432fdf324f2db2ebb0d08d6fe53f |
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| 출처 메모 | uspto-grants-2013_09 |
|---|
