참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Cyclopropanemethanol | HCID 75644 | — |
| 반응물 | 5-Amino-3-chloropyrazine-2-carbonitrile | HCID 21075392 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 5-Amino-3-(cyclopropylmethoxy)pyrazine-2-carbonitrile | HCID 59636353 | 83% |
반응 단계
To a solution of sodium hydride (93 mg, 3.882 mmol) in dioxane (4 mL) was added cyclopropylmethanol (280 mg, 3.882 mmol) dropwise. The solution was stirred for 30 minutes and then 5-amino-3-chloropyrazine-2-carbonitrile (300 mg, 1.941 mmol) was added and the reaction mixture heated at 90° C. for 14 hours. The reaction mixture was poured into aqueous HCl (1 M) and extracted with ethyl acetate. The aqueous layer was re-extracted with ethyl acetate. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated to dryness to give the title compound (305 mg, 1.605 mmol, 83%) which was used in subsequent steps without further purification. LC-MS (3) Rt=1.49 min; m/z (ESI+) 191 (M+H+).
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-99953e524ebb411787feb18a6c23ffa0 |
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| 출처 메모 | uspto-grants-2013_09 |
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