참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2,4-Dichloro-6-methoxy-3,5-triazine | HCID 19267 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-(4-(Difluoromethoxy)phenyl)ethan-1-amine | HCID 4962292 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 4-Chloro-N-{2-[4-(difluoromethoxy)phenyl]ethyl}-6-methoxy-1,3,5-triazin-2-amine | HCID 89619793 | 31.7% |
반응 단계
A solution of 1.8 g of 2,4-dichloro-6-methoxy-1,3,5-triazine in 40 ml of acetonitrile is cooled on an ice bath, 1.28 ml of DIPEA and then 1.68 g of 2-[4-(difluoromethoxy)phenyl]ethanamine are added and the mixture is stirred for 30 minutes. The reaction mixture is diluted by adding 100 ml of EtOAc and 50 ml of water, the phases are separated by settling, the organic phase is washed with saturated NaCl solution and dried over MgSO4, and the solvent is evaporated off under vacuum. The residue is taken up in DCM, the insoluble matter is filtered off and the filtrate is concentrated under vacuum. The residue is chromatographed on silica gel, eluting with a cyclohexane/EtOAc mixture in a gradient of from (95/5 v/v) to (80/20 v/v). 0.94 g of the expected compound is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09115121B2 |
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| 출처 데이터셋 | uspto-grants-2015_08 |
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| ORD ID | ord-b9beb49da07947d8883b89d17e513bab |
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| 출처 메모 | uspto-grants-2015_08 |
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