참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | (4-Nitrophenyl)methyl 4-chloro-3-oxobutanoate | HCID 20196963 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178520786 | HCID 178520786 | 97.6% |
반응 단계
In 100 ml of acetic acid is dissolved 50 g (0.184 mol, uncorrected for purity) of the crude p-nitrobenzyl γ-chloroacetoacetate obtained in 1), and the solution is cooled to 5° C. or lower, and a solution of 12.7 g (0.184 mol) of sodium nitrite in 50 ml of water is added dropwise thereto at 5° C. or lower over a period of an hour. After completion of the addition, the mixture is stirred for 30 minutes and poured into 600 ml of ice water and extracted with 300-ml and 200-ml portions of ethyl acetate. The organic layers are combined and washed with saturated aqueous sodium chloride, dried over sodium sulfate and concentrated to dryness to give 54.0 g of p-nitrobenzyl α-hydroxyimino-γ-chloroacetoacetate as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04673739 |
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| 출처 데이터셋 | uspto-grants-1987_06 |
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| ORD ID | ord-9ba81ae68fa24f05aed6a34b563f9905 |
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| 출처 메모 | uspto-grants-1987_06 |
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