참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | 4'-Bromoacetanilide | HCID 7683 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-(4-bromophenyl)-N-methylacetamide | HCID 4324567 | 90% |
반응 단계
Sodium hydride (101.5 mg, 2.33 mmol) (55% in paraffin liquid) was added to a solution of 249 mg (1.16 mmol) of the title compound produced in step (i) of Reference Example 7 in N,N-dimethylformamide (2.5 ml), and the mixture was stirred at room temperature for 30 min. Thereafter, methyl iodide was added, and the mixture was stirred at room temperature for 1 hr. The reaction was stopped by adding a saturated aqueous sodium hydrogencarbonate solution, and the reaction solution was extracted with ethyl acetate. The organic layer was washed with water and saturated brine in that order, was dried over anhydrous sodium sulfate, and was filtered. The filtrate was concentrated under the reduced pressure, and the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=2:1) to give 239 mg (yield 90%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07871982B2 |
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| 출처 데이터셋 | uspto-grants-2011_01 |
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| ORD ID | ord-2965961260a547e0839bf7d84898126b |
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| 출처 메모 | uspto-grants-2011_01 |
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