참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | N-benzyl-N-methylcarbamoyl chloride | HCID 10464985 | — |
| 반응물 | methyl 3-[(4,6-dimethoxypyrimidin-2-yl)oxy]picolinate N-oxide | HCID 14425903 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 15239969 | HCID 15239969 | 32% |
반응 단계
20 g (77.1 mmol) of methyl 3-[(4,6-dimethoxypyrimidin-2-yl)oxy]picolinate N-oxide, 15 g (116 mmol) of diisopropylethylamine and 46.2 g (308.2 mmol) of sodium iodide were suspended in 200 ml of acetonitrile and stirred at room temperature for 15 minutes. To this mixture, 21.2 g (115.4 mmol) of N-methyl-N-benzylcarbamoyl chloride dissolved in 20 ml of acetonitrile was added at room temperature. The mixture was refluxed. Foaming started at a temperature slightly lower than the boiling point, and such foaming terminated in about 30 minutes. The reaction was continued for further 10 minutes. The reaction solution was poured into water and extracted with ethyl acetate. The extract was washed with water, dried, concentrated and then purified by silica gel column chromatography to obtain the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05403816 |
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| 출처 데이터셋 | uspto-grants-1995_04 |
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| ORD ID | ord-cf59d4b1fa2d4d4481b66b5822abfd7e |
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| 출처 메모 | uspto-grants-1995_04 |
|---|