Methyl iodide → 3-[2-Chloro-4-fluoro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-1,2,3,6-tetrahydropyrimidin-1-yl)phenoxy]-2-(methoxycarbonylmethoxy)pyridine

HRID 1862230노트

반응식

HRID 1862230 반응식
[Cl:1][C:2]1[CH:20]=[C:19]([F:21])[C:18]([N:22]2[C:27](=[O:28])[CH:26]=[C:25]([C:29]([F:32])([F:31])[F:30])[NH:24][C:23]2=[O:33])=[CH:17][C:3]=1[O:4][C:5]1[C:6]([O:11][CH2:12][C:13]([O:15][CH3:16])=[O:14])=[N:7][CH:8]=[CH:9][CH:10]=1.[C:34](=O)([O-])[O-].[K+].[K+].CI>C(#N)C>[Cl:1][C:2]1[CH:20]=[C:19]([F:21])[C:18]([N:22]2[C:27](=[O:28])[CH:26]=[C:25]([C:29]([F:32])([F:31])[F:30])[N:24]([CH3:34])[C:23]2=[O:33])=[CH:17][C:3]=1[O:4][C:5]1[C:6]([O:11][CH2:12][C:13]([O:15][CH3:16])=[O:14])=[N:7][CH:8]=[CH:9][CH:10]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 11430Potassium CarbonateHCID 186192103-{2-Chloro-4-fluoro-5-[2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine

생성물 1

HCID 120567393-[2-Chloro-4-fluoro-5-(3-methyl-2,6-dioxo-4-trifluoromethyl-1,2,3,6-tetrahydropyrimidin-1-yl)phenoxy]-2-(methoxycarbonylmethoxy)pyridine수율 94.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a mixture of 0.10 g of 3-{2-chloro-4-fluoro-5-[2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine, 1 ml of acetonitrile and 31 mg of potassium carbonate, 32 mg of methyl iodide was added to the mixture, and the mixture was stirred at room temperature for 1.5 hours. 64 mg of methyl iodide was added to the mixture, and the mixture was stirred at 50° C. for 1 hour. The mixture was filterated, and the filterate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 97 mg of 3-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-(methoxycarbonyl)methoxypyridine [present compound 7-7].

후처리

  1. additionwas added to the mixture
  2. stirringthe mixture was stirred at 50° C. for 1 hour
  3. concentrationthe filterate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c1a1f95af5e040f88a159a5c5575daf5
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06537948B1

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