참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | 3-(Cyclopropylmethoxy)-4-(difluoromethoxy)benzaldehyde | HCID 18973698 | — |
| 반응물 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 생성물 | 3-(Cyclopropylmethoxy)-4-(difluoromethoxy)benzoic acid methyl ester | HCID 12136840 | 52% |
반응 단계
873 g of 3-(cyclopropylmethoxy)-4-(difluoromethoxy)-benzaldehyde (3.61 mol) were dissolved in MeOH (4.4 L), then solid Oxone® (1.86 Kg, 6.06 mol) was added portion-wise in 1 hour, and the solution was stirred and warmed to 55 to 60° C. for 2 hours. The solvent was concentrated under vacuum to 1.6 L and water (7 L) was added. The resulting heterogeneous solution was stirred at 50 to 55° C., then toluene (3 L) was added, and the biphasic mixture vigorously stirred. Aqueous phase was discharged and the organic one was washed with water (3 L). The solvent was concentrated under vacuum to 2 to 3 volumes, and the obtained solution warmed to 80 to 90° C. n-Heptane (5.5 L) was slowly added. The mixture was cooled to −10° C., and the suspension was stirred at −10° C. over-night. The solid was filtered on a Buchner funnel and washed with n-heptane (1 L). The obtained yellow solid was dried under vacuum at room temperature. (yield 52%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09434691B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-c1d41047786a48178e676e36ef809d32 |
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| 출처 메모 | uspto-grants-2016_09 |
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