참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chloral alcoholate | HCID 10587 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 반응물 | 4-Bromo-2-methoxyaniline | HCID 459257 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N-(4-bromo-2-methoxyphenyl)-2-(hydroxyimino)acetamide | HCID 117668132 | 68% |
반응 단계
Hydroxylamine hydrochloride (6.67 g, 96 mmol) in water (15 mL) was added to a suspension of 2,2,2-trichloro-1-ethoxyethanol (6.96 g, 36 mmol) and sodium sulfate (38.3 g, 270 mmol) in water (45 mL) and 2N HCl (30 mL). The mixture was stirred at 60° C. for 20 min. 4-Bromo-2-methoxybenzenamine (6.06 g, 30 mol) in 2N HCl (30 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 the title compound (5.55 g, crude, 68% yield). This material was used in the next step without further purification. MS (ESI) m/e [M+1]+ 273, 275.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09393232B2 |
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| 출처 데이터셋 | uspto-grants-2016_07 |
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| ORD ID | ord-93b3f8b4e035460eaa558faf2692cc4c |
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| 출처 메모 | uspto-grants-2016_07 |
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