참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 6-Methoxy-1,2,3,4-tetrahydroisoquinoline | HCID 39356 | — |
| 반응물 | 5-(Chloromethyl)-2-methylpyrimidin-4-amine--hydrogen chloride (1/1) | HCID 21473611 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-(6-methoxy-3,4-dihydro-1H-isoquinolin-2-ylmethyl)-2-methyl-pyrimidin-4-ylamine | HCID 21473698 | 22.2% |
반응 단계
A suspension of 0.80 g (0.00412 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride in 17 ml of dimethylformamide was treated with 1.7 ml (0.0124 mol) of triethylamine and 0.87 g (0.0053 mol) of 6-methoxy-1,2,3,4-tetrahydro-isoquinoline and the mixture was stirred at room temperature under argon for 3 hours. The mixture was completely freed from the solvents and the residue was triturated in 20 ml of water. The resulting crystals were filtered off under suction, chromatographed over silica gel with dichloromethane/methanol 9:1 as the eluent and recrystallized from ethyl acetate/n-hexane. 0.26 g (22%) of 5-(6-methoxy-3,4-dihydro-1H-isoquinolin-2-ylmethyl)-2-methyl-pyrimidin-4-ylamine was obtained as white crystals; m.p. 142°-143°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05688798 |
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| 출처 데이터셋 | uspto-grants-1997_11 |
|---|
| ORD ID | ord-49d977aebe9445428ad63540d468cc9e |
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| 출처 메모 | uspto-grants-1997_11 |
|---|
