참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Dimepranol | HCID 37511 | — |
| 반응물 | 5-Amino-3-chloropyrazine-2-carbonitrile | HCID 21075392 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 5-Amino-3-(1-(dimethylamino)propan-2-yloxy)pyrazine-2-carbonitrile | HCID 59636328 | — |
반응 단계
1-(Dimethylamino)propan-2-ol (187 mg, 1.81 mmol) was added to a stirred suspension of sodium hydride (123 mg, 60% in mineral oil, 1.81 mmol) in 1,4-dioxane. After 30 minutes, 5-amino-3-chloropyrazine-2-carbonitrile (140 mg, 0.906 mmol) was added. The vial was capped and the reaction mixture was heated to 100° C. overnight. The reaction mixture was concentrated, diluted with methanol and adsorbed onto an SPE (TsOH) cartridge (pre-conditioned with methanol). The cartridge was rinsed with methanol and the product was eluted with 2 M NH3 in methanol. The basic fractions were concentrated to give the title compound as an orange oil which was used without further purification (79.2 mg, 0.358 mmol, 40%). LC-MS (1) Rt=1.33 m/z (ESI+) 222 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08530468B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-29abdb38ca1942dba78ea6713ddfa4bd |
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| 출처 메모 | uspto-grants-2013_09 |
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