참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Methyl 5-bromo-3-(bromomethyl)pyridine-2-carboxylate | HCID 58171990 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-bromo-6-methyl-5H,6H,7H-pyrrolo[3,4-b]pyridin-7-one | HCID 59568581 | — |
반응 단계
Methylamine (2M in THF, 9.05 mL) was added to methyl 5-bromo-3-(bromomethyl)picolinate (Example 32, step (i), 1.036 g) in tetrahydrofuran (5 mL) at 20° C. under nitrogen. The resulting suspension was stirred at 70° C. for 30 min. The reaction mixture was cooled and filtered, and the filtrate evaporated to dryness to afford crude product. The crude product was purified by chromatography on silica eluting with ethyl acetate/dichloromethane (5:95 to 100:0). The solid collected during the filtration was dissolved in ethyl acetate and washed with water, extracted with dichloromethane, and then washed with saturated aqueous sodium bicarbonate solution and extracted again with dichloromethane. The combined organic extracts were dried over magnesium sulfate, and then combined with the chromatographed material to afford the sub-titled compound (0.372 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08193239B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-9e012ff2f8a64f07aa3e9c7fbc2587ef |
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| 출처 메모 | uspto-grants-2012_06 |
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