참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Piperidin-4-ol | HCID 79341 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-Chloro-4-((3-chloro-4-methoxybenzyl)amino)-6-phthalazinecarbonitrile | HCID 10451065 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | Yze9gcm2BB | HCID 9888568 | 85.6% |
반응 단계
10.0 g of 1-chloro-4-(3-chloro-4-methoxybenzyl)amino-6-cyanophthalazine was dissolved in 50 ml 1-methyl-2-pyrrolidone, then 43.32 g of 4-hydroxypiperidine and 10 ml diisopropylethylamine were added thereto, and the mixture was heated at 170° C. for 8 hr. After cooling, ethyl acetate was added thereto, and the mixture was washed 3 times with water and once with brine. After drying over anhydrous magnesium sulfate, the solvent was evaporated. The resulting residue was purified by silica gel column chromatography to give 10.1 g of 1-(4-hydroxypiperidino)-4-(3-chloro-4-methoxybenzyl)amino-6-cyanophthalazine as yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06699870B2 |
|---|
| 출처 데이터셋 | uspto-grants-2004_03 |
|---|
| ORD ID | ord-3c9d8bdbc7904fc7bd47f8bbdab1c318 |
|---|
| 출처 메모 | uspto-grants-2004_03 |
|---|
