참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Iodoethane | HCID 6340 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Carbonyl Sulfide | HCID 10039 | — |
| 반응물 | 2-[2-Chloro-4-(3,5-difluorophenoxy)phenoxy]ethylamine | HCID 15766489 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Ethyl 2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethylthiocarbamate | HCID 53835718 | 61% |
반응 단계
Into a mixture of 1.20 g of 2-[2-chloro-4-(3,5difluorophenoxy)phenoxy]ethylamine, 0.81 g of triethylamine and 20 ml of tetrahydrofuran, excesss of carbonyl sulfide gas was introduced with stirring at room temperature for 30 minutes. To the above mixture, there was added dropwise 0.75 g of ethyl iodide, and the resultant mixture was stirred at the same temperature for 24 hours. The reaction mixture was concentrated, and the residue was poured into 100 ml of water and extracted twice with 100 ml of ethyl acetate. The extracts were combined together, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 0.95 g of ethyl 2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethylthiocarbamate. Yield: 61%. nD21 : 1.5707.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05346920 |
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| 출처 데이터셋 | uspto-grants-1994_09 |
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| ORD ID | ord-b79b53482b844b0eadbbb594662579ea |
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| 출처 메모 | uspto-grants-1994_09 |
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