참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,6-Dichlorobenzaldehyde | HCID 6737 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Benzaldehyde, 2,6-dichloro-, oxime | HCID 91328 | 99.6% |
반응 단계
Sodium hydroxide 3N (3.14 L, 9.43 mol) is added dropwise to a stirred suspension of hydroxylamine hydrochloride (675.55 g, 9.43 mol) in 0.5 L of water at 0° C. To this mixture is added dropwise a suspension of 2,6-dichlorobenzaldehyde (1500 g, 8.57 mol) in 7.5 L of ethanol and the reaction is heated at 90° C. overnight. The mixture is cooled to room temperature and then, concentrated to dryness. The solid is triturated in a mixture of H2O/EtOH, 10:1 (4.4 L), filtered and dried under high vacuum at 45° C. overnight. 1621.78 g of title compound (99% yield) is obtained as a white solid. MS (m/e): 190 (M+1)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08153624B2 |
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| 출처 데이터셋 | uspto-grants-2012_04 |
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| ORD ID | ord-c3f0e80f6181496680572301a72f489f |
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| 출처 메모 | uspto-grants-2012_04 |
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