참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Picolinoyl Chloride Hydrochloride | HCID 135033 | — |
| 반응물 | 1-(4-(4-Amino-2-chlorophenyl)piperazin-1-yl)-2-methylpropan-1-one | HCID 936926 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(3-chloro-4-(4-isobutyrylpiperazin-1-yl)phenyl)picolinamide | HCID 42645025 | 18% |
반응 단계
According to Scheme 4 Step 3: Picolinoyl chloride hydrochloride (0.93 mmol, 178 mg) and Et3N (1.86 mmol, 0.26 mL) were added to a solution of 1-(4-(4-amino-2-chlorophenyl)piperazin-1-yl)-2-methylpropan-1-one (0.62 mmol, 175 mg) in DCM (3 mL) at 0° C. The reaction mixture was stirred at room temperature for 2 hours. The organic phase was washed with a saturated solution of NaHCO3. The aqueous phase was extracted with AcOEt. The organic phase was washed with brine, was dried over Na2SO4, was filtered and was concentrated under reduced pressure. The crude product was purified by flash chromatography over C18 column using water/ACN (60:40) as eluent to afford N-(3-chloro-4-(4-isobutyrylpiperazin-1-yl)phenyl)picolinamide (0.11 mmol, 42 mg, 18%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08524726B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-bf9a8f47cc0d45d592b8c2e6d4a9879b |
|---|
| 출처 메모 | uspto-grants-2013_09 |
|---|