참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-[4-(4-Fluorophenoxy)phenyl]ethan-1-amine | HCID 20991921 | — |
| 반응물 | HCID 178503543 | HCID 178503543 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 178518127 | HCID 178518127 | 53.1% |
반응 단계
2-Methylsulfanyl-5-pyrimidin-5-ylmethyl-1H-pyrimidin-4-one (30 mg, 0.128 mmol, 1 eq) and 2-[4-(4-Fluoro-phenoxy)-phenyl]-ethylamine (44.4 mg, 0.192 mmol, 1.5 eq) were dissolved in dry ethanol (300 μl) and stirred at 125° C. for overnight. Reaction mixture was evaporated and crude residue was sent to HPLC/MS Purification. After HPLC/MS purification combined fractions of desired product were collected and put on lyophilisation to obtain 2-{2-[4-(4-fluoro-phenoxy)-phenyl]-ethylamino}-5-pyrimidin-5-ylmethyl-1H-pyrimidin-4-one (0.068 mmol; yield: 53.1%, HPLC-MS/UV: [M+H]+=418.45; rt: 9.78 min; purity: 98%). 1H NMR (300 MHz; DMSO-d6) δ/ppm 2.75 (t, J=7.50 Hz, 2H), 3.39-3.49 (m, 2H), 3.51 (s, 2H), 6.46 (br.s, 1H), 6.90 (d, J=8.57 Hz, 2H), 6.97-7.05 (m 2H), 7.15-7.25 (m, 4H), 7.66 (s, 1H), 8.66 (s, 2H), 8.97 (s, 1H), 10.92 (br.s., 1H)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08637536B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_01 |
|---|
| ORD ID | ord-7400c84d4b8c49f1a1f6db6e7a2d9b98 |
|---|
| 출처 메모 | uspto-grants-2014_01 |
|---|