참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanamine, 2,2,2-trifluoro- | HCID 9773 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 반응물 | HCID 178493464 | HCID 178493464 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178493463 | HCID 178493463 | 62.3% |
반응 단계
Sodium triacetoxyborohydride (101 mg, 0.476 mmol, 3 equiv) was added to a suspension of 8-(2,6-dichloro-3,5-dimethoxy-phenyl)-quinoxaline-5-carboxylic acid (4-formyl-1H-imidazol-2-yl)-amide (75 mg, 0.159 mmol) and trifluoroethylamine (15 μl, 0.188 mmol), 1.18 equiv) in DCM (3 mL) at rt, under an argon atmosphere. The reaction mixture was stirred for 18 h at rt, quenched by addition of H2O and extracted with DCM. The organic phase was washed with a saturated aqueous solution of NaHCO3, dried (Na2SO4), filtered and concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 98:1:1) followed by trituration in Et2O to afford 55 mg of the title compound as a yellow solid: ES-MS: 555 [M+H]+; tR=3.78 min (System 1); TLC: Rf=0.55 (DCM/MeOH, 9:1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08536175B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-fd8d89651c0e41d991874d76a9329e3e |
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| 출처 메모 | uspto-grants-2013_09 |
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