참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-chloro-1-methyl-1H-pyrazole-5-carboxylic acid | HCID 670823 | — |
| 반응물 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 반응물 | HCID 67041977 | HCID 67041977 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 51035029 | HCID 51035029 | 1.5% |
반응 단계
Under an atmosphere of nitrogen, N—N-diisopropylethylamine (121 mg) and 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (TBTU, 120 mg) were added to a solution of 4-chloro-2-methyl-2H-pyrazole-3-carboxylic acid (50 mg, 0.31 mmol, Art-Chem B000148) in DMF (3 ml). After 30 min, 5-morpholin-4-yl-2-phenyl-imidazo[1,2-c]pyrimidin-7-ylamine (110 mg, 0.37 mmol) was added, and the black solution was stirred at r.t. overnight. The reaction mixture was taken up in ethyl acetate and washed with water. After drying (Na2SO4), the solvent was evaporated and the title compound (2 mg, 1.1%) was isolated by preparative, inverse-phase HPLC (Agilent Zorbax XdB-C18 column, time per run ˜7 min, flow rate 30 ml/min, solvent gradient H2O/CH3CN=95:5-5:95). MS (m/e)=438.2 [M+H+].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08017604B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_09 |
|---|
| ORD ID | ord-1f7b8e1780ef4b3b8442ffbb5b20cd29 |
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| 출처 메모 | uspto-grants-2011_09 |
|---|
