Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 4-(2-(5-bromo-2-fluorophenyl)pteridin-4-ylamino)-N-(3-(2-oxopyrrolidin-1-yl)propyl)nicotinamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | PyBOP | HCID 2724699 | — |
| 반응물 | 1-(2-Aminopropyl)-2-pyrrolidinone | HCID 16787003 | — |
| 반응물 | 4-[[2-(5-Bromo-2-fluorophenyl)pteridin-4-yl]amino]nicotinic Acid | HCID 57742374 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(2-(5-bromo-2-fluorophenyl)pteridin-4-ylamino)-N-(3-(2-oxopyrrolidin-1-yl)propyl)nicotinamide | HCID 11955790 | 30.2% |
반응 단계
Triethylamine (140 μL, 1.00 mmol) was slowly added to a solution of 4-[[2-(5-bromo-2-fluorophenyl)pteridin-4-yl]amino]nicotinic acid 16 (150 mg, 0.340 mmol), PyBOP (0.350 mg, 0.68 mmol), and 1-(β-aminopropyl)pyrrolidinone (97 mg, 0.68 mmol) in CH2Cl2 (10 mL). After 15 min at room temperature, the reaction mixture was evaporated and the residue purified by column chromatography (AcOEt/CH2Cl2, 2:1+1% triethylamine to AcOEt/CH2Cl2/MeOH, 7:2:1+1% triethylamine). The yellow powder was recrystallized from EtOH to give 58 mg of the title product 21 as yellow prisms (LCMS analysis).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09290502B2 |
| 출처 데이터셋 | uspto-grants-2016_03 |
| ORD ID | ord-702c0055a4154d8086e2321a7aa40a1f |
| 출처 메모 | uspto-grants-2016_03 |