참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Cyanogen Bromide | HCID 10476 | — |
| 반응물 | 2-(4,5-dihydro-1H-imidazol-2-yl)-6-methoxyaniline | HCID 58377357 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Triethylammonium bromide | HCID 2734074 | 296.1% |
| 생성물 | HCID 178488375 | HCID 178488375 | — |
반응 단계
2-(4,5-Dihydro-1H-imidazol-2-yl)-6-methoxyaniline (Step 3, 22.0 g, 115 mmol) and Et3N (48.1 mL, 345 mmol) were dissolved in CH2Cl2 (200 mL), cooled to 10° C. in an ice bath and cyanogen bromide (24.4 g, 230 mmol) was added portionwise. A slight exotherm was noted, and the reaction was stirred overnight. The reaction was concentrated under reduced pressure, then treated with EtOAc (150 mL) and concentrated under reduced pressure again. Finally, the residue was treated with Heptane and concentrated under reduced pressure to give the title compound as a mixture with Et3N.HBr (62 g, 99%): HPLC MS RT=1.08 min, MH+=217.1; 1H NMR (DMSO-d6+2 drops TFA-d) δ: 3.85 (3H, s), 4.09-4.16 (2H, m), 4.31-4.38 (2H, m), 7.23 (1H, t), 7.31 (1H, d), 7.57 (1H, dd).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08859572B2 |
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| 출처 데이터셋 | uspto-grants-2014_10 |
|---|
| ORD ID | ord-cbf1799c49494e7eaaac2cf948a53bb4 |
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| 출처 메모 | uspto-grants-2014_10 |
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