참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 2-Amino-3,6-dichloro-5-trifluoromethylpyridine | HCID 13064154 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Amino-3-chloro-6-methoxy-5-trifluoromethylpyridine | HCID 22101795 | — |
반응 단계
6.7 g (0.029 mol) of 2-amino-3,6-dichloro-5-trifluoromethylpyridine were added to a stirred mixture of 2.4 g (0.0377 mol) of 88% potassium hydroxide powder in 10 ml of methanol and 100 ml of dimethylformamide at 20° C. in the course of 5 minutes. The reaction mixture was now stirred for 89 hours at 130° C., with HPLC monitoring, a further 5 ml of methanol being added to the reaction mixture after 40 hours. After working-up in accordance with Example I.2., 0.3 g (4.6% of theory) of the title compound of ηD 24 =1.5143 was obtained in fractions 3 and 4. Fraction 5 contained 0.7 g (10% of theory) of 2-amino-3-chloro-6-dimethylamino-5-trifluoromethylpyridine (NMR 400 MHz, CDCl3 7.58 (pyridine), 2.95 (CH3)2N) and fractions 9-16 contained 1.1 g (16% of theory) of starting material. Other secondary components were found in the fractions which followed.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05750705 |
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| 출처 데이터셋 | uspto-grants-1998_05 |
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| ORD ID | ord-bf565feaf0ba45a9b9f926afdb023bec |
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| 출처 메모 | uspto-grants-1998_05 |
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