참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydroxylamine | HCID 787 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2'-Bromoacetophenone | HCID 75060 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 용매 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 생성물 | Ethanone, 1-(2-bromophenyl)-, oxime | HCID 818696 | 83% |
반응 단계
Combine 1-(2-bromo-phenyl)-ethanone (4.5 g, 22.6 mmol), 50% hydroxylamine in water (2.3 g, 69.6 mmol) and 1 mL of acetic acid in 15 mL of dioxane in a pressure vessel. Seal the vessel and heat the mixture in an oil bath for 3 h at 150° C. Cool the mixture to room temperature (RT). Dilute with chloroform/IPA (3/1), wash with water and aqueous saturated sodium chloride. Separate the layers and dry the organic layer over sodium sulfate. Concentrate in vacuo to give the crude product. Purify by column chromatography (20% THF in dichloromethane (DCM) to give the title compound (4.0 g, 83%). MS (ES) m/z 214/216 [M+1]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08063035B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_11 |
|---|
| ORD ID | ord-7cf66e0c305c43e4924391d5750a8c37 |
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| 출처 메모 | uspto-grants-2011_11 |
|---|
