참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Aminocyclohexanol | HCID 23286 | — |
| 반응물 | 4-(2-Chloroethyl)phenyl methyl ether | HCID 87513 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(4-Methoxyphenethylamino)cyclohexanol | HCID 60714650 | — |
반응 단계
Mix (±)-2-aminocyclohexanol (1.5227 g, 13.2 mmol), K2CO3 (4.56 g, 33.0 mmol), and 1-(2-chloroethyl)-4-methoxybenzene (2.0 mL, 13.2 mmol) in DMF (30 mL). Heat at 100° C. for 24 hours. Cool down to room temperature and filtrate with MeOH wash. Concentrate and remove DMF azeotropically with xylenes. Take up the residue in CH2C2 and H2O (100 mL each). Separate the layers and extract the aqueous layer with CH2Cl2 (2×100 mL). Wash the organic layers with H2O and brine (100 mL each). Dry the combined organic layers over MgSO4, concentrate and purify by flash chromatography, eluting with 50:45:5 EtOAc/CH2Cl/2.0 M NH3 in MeOH to afford 2-(4-methoxyphenethylamino)cyclohexanol. (1.38 g, 42%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07560463B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
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| ORD ID | ord-7b727e9032f0430099b8f30e0642387b |
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| 출처 메모 | uspto-grants-2009_07 |
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