참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dibromoethane | HCID 7839 | — |
| 반응물 | Diisopropylamine | HCID 7912 | — |
| 반응물 | 2-(6-Bromopyridin-2-yl)acetonitrile | HCID 642864 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-(6-Bromopyridin-2-YL)cyclopropanecarbonitrile | HCID 59525675 | — |
반응 단계
n-Butyllithium (6.66 ml, 10.7 mmol) was added to a cooled (0° C.) solution of diisopropylamine (1.52 ml, 10.7 mmol) in THF (10 mL) and maintained at 0° C. for 30 minutes. The reaction was then cooled to −78° C. and a solution of (6-bromopyridin-2-yl)acetonitrile (Example 235, Step 1) (1 g, 5.08 mmol) in tetrahydrofuran (10 mL) was added dropwise. The reaction was maintained at −78° C. for 1 hour, and then 1,2-dibromoethane (0.92 ml, 10.7 mmol) was added. The reaction was allowed to warm to room temperature and maintained at room temperature for 3 days. The mixture was then diluted with water and ethyl acetate and the layers were separated. The organic layer was dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography afforded the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08367706B2 |
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| 출처 데이터셋 | uspto-grants-2013_02 |
|---|
| ORD ID | ord-8105fbe7f4cc49b7b24d5d28a2c262f1 |
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| 출처 메모 | uspto-grants-2013_02 |
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