참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-Isopropyl-homopiperazine | HCID 12236513 | — |
| 반응물 | Methyl 2-chloropyrimidine-5-carboxylate | HCID 12627752 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66589803 | HCID 66589803 | 79.3% |
반응 단계
A solution of methyl 2-chloropyrimidine-5-carboxylate (209 mg, 1.21 mmol) in dichloromethane (4.00 ml) was added to a stirred solution of 1-propan-2-yl-1,4-diazepane (172 mg, 1.21 mmol) and N-ethyl-N-propan-2-ylpropan-2-amine (0.523 ml, 3.02 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-propan-2-yl-1,4-diazepan-1-yl)pyrimidine-5-carboxylate (267 mg, 79%) as a cream oil which crystallised on standing. 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-034e917bbaf943f7aa112512ea8a04e5 |
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| 출처 메모 | uspto-grants-2010_06 |
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