참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| 반응물 | 4-Aminobenzyl alcohol | HCID 69331 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | [4-(2-Amino-6-chloro-pyrimidin-4-yl-amino)-phenyl]-methanol | HCID 86004324 | 63% |
반응 단계
A mixture of 4,6-dichloro-pyrimidin-2-yl-amine (6.6 g, 40 mmol), 4-aminobenzyl alcohol (8.0 g, 65 mmol) and N,N-diisopropylethylamine (15 ml) in ethanol (200 ml) was heated under reflux for 72 hours. Concentration under reduced pressure provided a solid which was stirred with 1.0 M hydrochloric acid (200 ml) for 1 hour, filtered, dried under reduced pressure, stirred with ethyl acetate (200 ml) for 2 hours, filtered, and dissolved in methanol (300 ml). Aqueous sodium carbonate solution (1.0 M, 50 ml) was added. After stirring for 2 hours, volatiles were evaporated under reduced pressure and water (200 ml) was added. Filtration and drying provided [4-(2-amino-6-chloro-pyrimidin-4-yl-amino)-phenyl]-methanol (6.3 g, 63% yield) as a white powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07419984B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-753ba51b07e845fc9cfead58758f27e0 |
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| 출처 메모 | uspto-grants-2008_09 |
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