참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | Ethyl difluoro(pyridin-2-yl)acetate | HCID 10631894 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 2,2-Difluoro-2-(pyridin-2-YL)ethanol | HCID 9942216 | — |
반응 단계
Ethyl difluoro(pyridin-2-yl)acetate (G) obtained in step 1 (20 g) and 120 mL of ethanol were added, and 4 g of sodium borohydride was added to the reaction mixture over a period of 30 minutes at 0-5° C. The reaction mixture was stirred for 1 hour at 0-10° C. After completion of the reaction, the RM was quenched by adding saturated ammonium chloride solution at 0-5° C. and the volume of reaction mixture was reduced to half by distilling under vacuum. The solution was basified with 50% NaOH solution and extracted with MTBE. The organic layer was washed with a brine solution, dried over sodium sulphate and distilled under vacuum. The crude material was dissolved in 40 mL MTBE, 70 mL of n-hexane at 0-10° C. was added, and the RM was stirred for 30 minutes. The solid obtained was filtered and washed with hexane, resulting in pure product. (Yield=11 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541580B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-794d04e37e544a3693ded795a30aadb0 |
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| 출처 메모 | uspto-grants-2013_09 |
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