참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Methyl 2-chloropyrimidine-5-carboxylate | HCID 12627752 | — |
| 반응물 | 1-Cyclopropylhexahydro-1H-1,4-diazepine | HCID 20348476 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66589974 | HCID 66589974 | 97.3% |
반응 단계
A solution of methyl 2-chloropyrimidine-5-carboxylate (200 mg, 1.16 mmol) in dichloromethane (4.00 mL) was added to a stirred solution of 1-cyclopropyl-1,4-diazepane (247 mg, 1.16 mmol) and N-ethyl-N-propan-2-ylpropan-2-amine (0.902 mL, 5.22 mmol) in dichloromethane (4.00 mL) at 25° C. The resulting solution was stirred at ambient temperature for 18 h. The reaction mixture was evaporated to dryness and redissolved in MeOH (20 mL) and the crude product was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH and evaporated to dryness to afford methyl 2-(4-cyclopropyl-1,4-diazepan-1-yl)pyrimidine-5-carboxylate (312 mg, 97%) as a cream solid. This was used directly with no further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07737149B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-31947986d7cc4c65a57bef9e7bfc1e4b |
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| 출처 메모 | uspto-grants-2010_06 |
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