참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzylamine | HCID 7504 | — |
| 반응물 | Potassium Cyanide | HCID 9032 | — |
| 반응물 | Ethyl 1-formylcyclopropanecarboxylate | HCID 9964122 | — |
| 반응물 | Sodium Bisulfite | HCID 23665763 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(1-Benzylamino-1-cyanomethyl)-1-ethoxycarbonylcyclopropane | HCID 15391046 | 79% |
반응 단계
An eggplant type flask was charged with 501 mg of ethyl 1-formylcyclopropane-1-carboxylate and 2 ml of water to which were further added 1.13 g of sodium hydrogen sulfite and 345 mg of potassium cyanide. Thereto was added dropwise 564 mg of benzylamine dissolved in 5 ml of ethanol at room temperature, followed by 2.5 hours of stirring the reaction solution at 50° C. After confirming completion of the reaction, the reaction solution was mixed with ice water and extracted with ethyl acetate. Next, the resulting organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and, after removing insoluble matter by filtration, concentrated under a reduced pressure. Thereafter, the resulting residue was subjected to a silica gel column chromatography (hexane:ethyl acetate=3:1) to obtain 717 mg (79%) of the title compound in the form of colorless oil. Spectrum data of the thus obtained oily product coincided with those of the compound of Inventive Example 2.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05856518 |
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| 출처 데이터셋 | uspto-grants-1999_01 |
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| ORD ID | ord-aa72cbc4646e4f62a6622ce558e7dbc7 |
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| 출처 메모 | uspto-grants-1999_01 |
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