참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 4-Bromophenylhydrazine hydrochloride | HCID 12157 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | Ethyl 6-oxo-6-phenylhexanoate | HCID 3681727 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | ethyl (6E)-6-[(4-bromophenyl)hydrazinylidene]-6-phenylhexanoate | HCID 88116819 | 98.2% |
반응 단계
A mixture of 1.91 g (8.55.10−3 mol) of 4-bromophenylhydrazine hydrochloride and 0.73 g (8.9.10−3 mol) of sodium acetate in 17 ml of water is prepared and 2.05 ml (35.8.10−3 mol) of acetic acid are added. This mixture is subsequently heated to 70° C., with stirring, and a suspension of 2.0 g (8.54.10−3 mol) of ethyl ε-oxobenzenehexanoate in 27 ml of water is then added slowly. The reaction mixture is stirred at 70-80° C. for 45 min and then at room temperature for 12 hours, after which it is extracted with 2 times 50 ml of ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate and concentrated under reduced pressure to give 3.38 g of the expected compound, which is used directly in the next step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06605633B1 |
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| 출처 데이터셋 | uspto-grants-2003_08 |
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| ORD ID | ord-c4b25c39ebd44f3e865c7db8db138490 |
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| 출처 메모 | uspto-grants-2003_08 |
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