참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Mci-186 | HCID 4021 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 생성물 | 1-Phenyl-3-methyl-4-formyl-5-pyrazolone | HCID 205106 | 65% |
반응 단계
29 Grams of 3-methyl-1-phenyl-2-pyrazoline-5-one and 40 ml of dimethylformamide were charged into a 200-ml three-necked flask, stirred and cooled to 0° C. in an ice-acetone bath. Then, 18.5 g of phosphorus oxychloride (POCl3) was placed in a dropping funnel, and while it was maintained at 10 to 20° C., it was dropwise added. After the addition, the mixture was heated for 1 hour, then, a reaction mixture was poured into 600 ml of ice water, and the mixture was allowed to stand for one day and night. A crystal was recovered by suction filtration, fully washed with water and dried to give the captioned compound. Yield: 65%, Melting point: 178-180° C. (documented value: 174-175° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06310215B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_10 |
|---|
| ORD ID | ord-d6ce87e9240240ba9fb72e807c70bda7 |
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| 출처 메모 | uspto-grants-2001_10 |
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