참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,1-Dichloroethane | HCID 6365 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | N-Hydroxypropionimidamide | HCID 4092053 | — |
| 반응물 | HCID 54397424 | HCID 54397424 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 54348717 | HCID 54348717 | 34.5% |
반응 단계
Dichloroethane (5 ml), thionyl chloride (0.65 g, 5.5 mmol) and N,N-dimethylformamide (0.05 ml) were added to 2-(2,5-dimethylphenoxymethyl)-α-methoxyiminophenylacetic acid (1.57 g, 5 mmol), and the mixture was stirred under reflux for 2 hours. After completion of the reaction, the mixture was concentrated under reduced pressure, pyridine (3 ml) and 1-hydroxyimino-1-propylamine (0.88 g, 10 mmol) were added to the residue, and the mixture was stirred under reflux for 0.5 hours. After completion of the reaction, ether (150 ml) was added, and the mixture was washed with 1N hydrochloric acid (150 ml) twice. The ether layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate/n-hexane) and recrystallized from ethyl acetate/n-hexane to give 2-(2,5-dimethylphenoxymethyl)phenyl 3-ethyl-1,2,4-oxadiazol-5-yl ketone O-methyloxime (0.63 g, 34.5%) as colorless crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06268312B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_07 |
|---|
| ORD ID | ord-818edd6a6ca140e39c2de4bea2a9049e |
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| 출처 메모 | uspto-grants-2001_07 |
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