참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methyl-4-nitrobenzenesulfonate | HCID 22582 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 7-bromo-3-(3-chlorophenyl)isoquinolin-1(2H)-one | HCID 69928893 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 7-bromo-3-(3-chlorophenyl)-2-methylisoquinolin-1(2H)-one | HCID 69928548 | 50.2% |
반응 단계
7-Bromo-3-(3-chlorophenyl)isoquinolin-1(2H)-one (Intermediate 23A) (0.1 g, 0.299 mmol) was dissolved in THF (4 mL), under an atmosphere of nitrogen. Sodium hydride (0.018 g, 0.448 mmol) was added and reaction stirred for 30 minutes. The reaction was then cooled using an ice bath and methyl 4-nitrobenzenesulfonate (0.065 g, 0.299 mmol) was added. The reaction was allowed to warm to room temperature and left to stir overnight. Water was added to the reaction mixture and extracted with EtOAC (×2). The organics were combined and washed with brine, dried (MgSO4) filtered and concentrated under reduced pressure. The mixture was purified on silica (25 g column on Isolera 4) eluting with 0-10% methanol in dichloromethane to afford 7-bromo-3-(3-chlorophenyl)-2-methylisoquinolin-1(2H)-one (51 mg, 0.15 mmol).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841289B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-d964deca7655450c9db475cc20959061 |
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| 출처 메모 | uspto-grants-2014_09 |
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