Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Hydroxybenzotriazole → N-[4-(4-Amino-pyrazolo[3,4-d]pyrimidin-1-yl)-phenyl]-3-methoxy-propionamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 3-Methoxypropionic acid | HCID 134442 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 1-(4-Amino-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine | HCID 11995960 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-[4-(4-Amino-pyrazolo[3,4-d]pyrimidin-1-yl)-phenyl]-3-methoxy-propionamide | HCID 11996397 | 20% |
반응 단계
Title compound 11A, 1-(4-amino-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (37 mg, 1.1 eq, 0.16 mmol) was added to a solution of 3-methoxypropionic acid (15.5 mg, 1.0 eq, 0.15 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (25 mg, 1.0 eq, 0.16 mmol), 1-hydroxybenzotriazole (20 mg, 1.0 eq, 0.15 mmol) in DMF (1 ml) which had been stirred for 10 minutes under an inert atmosphere. The reaction was stirred at room temperature for 18 hours, after which methanol (1 ml) was added, and solvent was removed in vacuo. The resultant solid was washed with water and purified by semi-preparative HPLC to yield the title compound as a white solid (9.3 mg, 0.03 mmol, 20%). LCMS: [M+H]+=313, Rt=1.31 min, 100% purity.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08071607B2 |
| 출처 데이터셋 | uspto-grants-2011_12 |
| ORD ID | ord-4ddad08c9e9b4e55a98e2ac84e8df074 |
| 출처 메모 | uspto-grants-2011_12 |