참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | 3-Chloro-4-fluorobenzonitrile | HCID 145525 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Methyl 3-Amino-4-methoxybenzoate | HCID 2734814 | — |
| 생성물 | HCID 178498285 | HCID 178498285 | 45% |
반응 단계
Anhydrous p-toluene sulfonic acid (10 g, 52.57 mmol) was melted at 120° C. and 3-amino-4-methoxy benzoic acid methyl ester (3.88 g, 21.44 mmol) obtained in step 1 of Preparation Example 1 and 3-chloro-4-fluorobenzonitrile (5.0 g, 32.14 mol) were added thereto and stirred at 160° C. for 8 hours. The resulting solution was cooled to room temperature and the reaction was stopped by adding NaHCO3 thereto. The resulting mixture was extracted with ethyl acetate, the extract was dried over MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (3.24 g, 9.62 mmol) in a yield of 45%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07179832B2 |
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| 출처 데이터셋 | uspto-grants-2007_02 |
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| ORD ID | ord-0f3630fd6bd54e7a832327e814aa6609 |
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| 출처 메모 | uspto-grants-2007_02 |
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