참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chlorite | HCID 23668197 | — |
| 반응물 | Monosodium phosphate | HCID 23672064 | — |
| 반응물 | 2-Cyclopropyl-4,6-bis-trifluoromethyl-benzaldehyde | HCID 58167762 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | tert-Butanol | HCID 6386 | — |
| 용매 | 2-Methyl-2-butene | HCID 10553 | — |
| 생성물 | 2-Cyclopropyl-4,6-bis-trifluoromethyl-benzoic acid | HCID 58167765 | — |
반응 단계
Crude 2-cyclopropyl-4,6-bis-trifluoromethyl-benzaldehyde (intermediate 0, 1.01 g, 3.58 mmol) was dissolved in 8.5 mL tert-butylalcohol and 4.5 mL 2-methyl-2-butene. At 0° C. a solution of sodium chlorite (340 mg, 3.76 mmol) and sodium dihydrogenphosphat (451 mg, 3.76 mmol) in 3 mL water was added. The reaction mixture was stirred at room temperature overnight. The solvents were evaporated off. The residue was taken up in 1N NaOH and extracted twice with tert-butyl methyl ether. The aqueous phase was adjusted to pH 2 by addition of 25% HCl and extracted twice with tert-butyl methyl ether. The combined organic phases were dried on sodium sulfate, filtered and evaporated. The crude material, off-white solid (1.01 g, 54%) was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08524909B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-2e1ade2d28d9474d8de193c5da09005f |
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| 출처 메모 | uspto-grants-2013_09 |
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