참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Ephedrine Hydrochloride | HCID 65326 | — |
| 반응물 | HCID 178432852 | HCID 178432852 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178433158 | HCID 178433158 | 15.1% |
반응 단계
To a 5-mL, Wheaton vial were added 4-chloro-2-methyl-6-phenylpyrrolo[3,2-d]pyrimidine (Example 1 (e)) (100 mg, 0.41 mmol) and ephedrine hydrochloride (Aldrich Chemical Company) (410 mg, 2.1 mmol), followed by addition of a solution of potassium carbonate (0.71 g, 5.1 mmol) in water (2.5 mL). The reaction mixture was stirred at 120° C. for 20 h, allowed to cool to room temperature and extracted with CH2Cl2. The organic layer was dried over Na2SO4, concentrated in vacuo to give a brown residue, which was purified by flash chromatography on silica gel with 1:1 EtOAc/hexanes as eluant to give 23 mg (15%) of the title compound as a tan solid. 1H NMR (DMSO-d6; 400 MHz): d 1.21 (d, 3, J=6.8), 2.42 (s, 3), 3.21 (s, 3), 4.91 (m, 1), 5.02 (m, 1), 5.87 (br s, 1), 6.69 (s, 1), 7.18-7.85 (m, 10), 10.73 (br s, 1). MS m/z: 373 (M+1), 371 (M−1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06583154B1 |
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| 출처 데이터셋 | uspto-grants-2003_06 |
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| ORD ID | ord-24279bd221624d47a4553d839a01e33d |
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| 출처 메모 | uspto-grants-2003_06 |
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