참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Tert-Butyl nitrite | HCID 10906 | — |
| 반응물 | 3-Amino-2,4,5-trifluorobenzoic acid | HCID 2735946 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-Chloro-2,4,5-trifluorobenzoic Acid | HCID 2734269 | — |
반응 단계
9.3 g of anhydrous cuprous chloride and 8.8 g of tert-butyl nitrite were added to 150 ml of acetonitrile and under stirring and heating at 60° C. 11 g of 3-amino-2,4,5-trifluorobenzoic acid 26 (a commercial product) was added. The mixture was stirred for 20 minutes. After cooling, 500 ml of 15% hydrochloric acid was added and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and the solvent was then removed under reduced pressure. Finally the residue was subjected to silica gel (100 g) column chromatography using chloroform as an eluent. The procedure gave 8.4 g of 3-chloro-2,4,5-trifluorobenzoic acid 27 as colorless needles.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05508428 |
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| 출처 데이터셋 | uspto-grants-1996_04 |
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| ORD ID | ord-a1b717582ed3483bbb765584c1cc9543 |
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| 출처 메모 | uspto-grants-1996_04 |
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