참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 4-Chloro-6-methylpyrimidine | HCID 581796 | — |
| 반응물 | (4-Phenyl-4,5,6,7-tetrahydro-benzothiazol-2-yl)-piperidin-4-yl-amine dihydrochloride | HCID 86656698 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 58397898 | HCID 58397898 | — |
반응 단계
(4-Phenyl-4,5,6,7-tetrahydro-benzothiazol-2-yl)-piperidin-4-yl-amine dihydrochloride (77.3 mg, 0.2 mmol) was suspended in tetrahydrofurane (2 mL). At 0° C. N,N-diisopropylethylamine (110 1, 0.64 mmol) was added at room temperature under nitrogen and stirring. To the yellow solution 4-chloro-6-methylpyrimidine (28.9 mg, 0.22 mmol) was added and the reaction was stirred at room temperature over night. The reaction was heated to reflux over night and then heated with N-methylpyrrolidone in a microwave oven to 200° C. for 30 minutes. Water was added and the reaction was extracted twice with diethyl ether. The combined organic layers were washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using a gradient from EtOAc to EtOAc/EtOH 9:1 (v/v) as eluent. The title compound was obtained as a light yellow solid (55 mg, 68%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08486967B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-b5a8904add3e45839fa2c47615c53cbf |
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| 출처 메모 | uspto-grants-2013_07 |
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