참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2-Bromopyridine 1-oxide hydrochloride | HCID 2724044 | — |
| 반응물 | 2,2-Dimethyl-6-nitro-3,4-dihydro-2H-benzo[B][1,4]oxazine | HCID 10727057 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(3,4-Dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazin-4-yl)pyridine N-oxide | HCID 131974 | — |
반응 단계
In 10 ml of N,N-dimethylformamide was dissolved 2.66 g of 3,4-dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazine followed by addition of 1.02 g of sodium hydride (60% in oil) and the mixture was stirred at room temperature for 30 minutes. Then, 2.77 g of 2-bromopyridine N-oxide hydrochloride was added with ice-cooling and, after the evolution of heat had subsided, the mixture was stirred at room temperature for 2 hours. The reaction mixture was then poured in water and extracted with ethyl acetate. The organic layer was separated and dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure and the residue was chromatographed on a silica gel column using chloroform as the eluent to give crude 2-(3,4-dihydro-2,2-dimethyl-6-nitro-2H-1,4-benzoxazin-4-yl)pyridine N-oxide.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05420126 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-43bd8fdba5d64894acdd9bc217ce5490 |
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| 출처 메모 | uspto-grants-1995_05 |
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