Hydrochloric Acid → 3-{2-Chloro-4-fluoro-5-[2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine

HRID 1862339노트

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HRID 1862339 반응식
[H-].[Na+].[NH2:3]/[C:4](/[C:11]([F:14])([F:13])[F:12])=[CH:5]\[C:6]([O:8]CC)=O.[Cl:15][C:16]1[C:21]([O:22][C:23]2[C:24]([O:29][CH2:30][C:31]([O:33][CH3:34])=[O:32])=[N:25][CH:26]=[CH:27][CH:28]=2)=[CH:20][C:19]([N:35]=[C:36]=[O:37])=[C:18]([F:38])[CH:17]=1.Cl>CN(C)C=O>[Cl:15][C:16]1[CH:17]=[C:18]([F:38])[C:19]([N:35]2[C:6](=[O:8])[CH:5]=[C:4]([C:11]([F:12])([F:13])[F:14])[NH:3][C:36]2=[O:37])=[CH:20][C:21]=1[O:22][C:23]1[C:24]([O:29][CH2:30][C:31]([O:33][CH3:34])=[O:32])=[N:25][CH:26]=[CH:27][CH:28]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 5702529Ethyl 3-amino-4,4,4-trifluorocrotonateHCID 186192764-Chloro-2-fluoro-5-{2-(methoxycarbonyl)methoxy-3-pyridyloxy}phenyl isocyanate

생성물 1

HCID 186192103-{2-Chloro-4-fluoro-5-[2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

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온도
0 °C

실험 절차

To a mixture of 1 ml of N,N-dimethylformamide and 26 mg of sodium hydride, a solution of 126 mg of ethyl 3-amino-4,4,4-trifluorocrotonate in 1 ml of N,N-dimethylformamide was added and the mixture was stirred at 0° C. Thereafter, to the reaction mixture was added a mixture of 266 mg of 4-chloro-2-fluoro-5-{2-(methoxycarbonyl)methoxy-3-pyridyloxy}phenyl isocyanate and 1 ml of N,N-dimethylformamide at the same temperature, and the mixture was stirred over night at room temperature. The reaction solution was poured into a mixture of hydrochloric acid and ice water, and to obtain 3-{2-chloro-4-fluoro-5-[2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine.

후처리

  1. additionThereafter, to the reaction mixture was added
  2. stirringthe mixture was stirred over night at room temperature

출처 및 근거

ORD 기록
ord-6732037b723c423f8924de54a13ed7d3
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06537948B1

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