참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Chloro-4-fluoroaniline | HCID 9708 | — |
| 반응물 | Chloral alcoholate | HCID 10587 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N-(3-chloro-4-fluorophenyl)-2-(hydroxyimino)ethanamide | HCID 73843641 | 90% |
반응 단계
Hydroxylamine hydrochloride (22.24 g, 320 mmol) in water (50 mL) was added to a suspension of 2,2,2-trichloro-1-ethoxyethanol (23.21 g, 120 mmol) and sodium sulfate (128 g, 900 mmol) in water (150 mL) and 2N HCl (100 mL). The mixture was stirred at 60° C. for 20 min. 3-Chloro-4-fluoroaniline (14.56 g, 100 mmol) in 2N HCl (100 mL) was added, and the mixture was heated to 90° C. for 2 h. The mixture was cooled to room temperature. The solid was collected by filtration, washed with water, and air dried to afford N-(3-chloro-4-fluorophenyl)-2-(hydroxyimino)ethanamide (19.45 g, 90% yield). This material was used in the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08658636B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-eef063229fc84486aa3ffca5018a22bf |
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| 출처 메모 | uspto-grants-2014_02 |
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