Methanol → Methyl 2-[2-({2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidine-1-yl]phenoxy}methyl)phenoxy]propionate

HRID 432559ノート

反応式

HRID 432559 の反応式
CO.[Cl:3][C:4]1[CH:25]=[C:24]([F:26])[C:23]([N:27]2[C:32](=[O:33])[CH:31]=[C:30]([C:34]([F:37])([F:36])[F:35])[N:29]([CH3:38])[C:28]2=[O:39])=[CH:22][C:5]=1[O:6][CH2:7][C:8]1[CH:21]=[CH:20][CH:19]=[CH:18][C:9]=1[O:10][CH:11]([CH3:17])[C:12]([O:14][CH2:15]C)=[O:13].C[O-].[Na+]>Cl>[Cl:3][C:4]1[CH:25]=[C:24]([F:26])[C:23]([N:27]2[C:32](=[O:33])[CH:31]=[C:30]([C:34]([F:35])([F:36])[F:37])[N:29]([CH3:38])[C:28]2=[O:39])=[CH:22][C:5]=1[O:6][CH2:7][C:8]1[CH:21]=[CH:20][CH:19]=[CH:18][C:9]=1[O:10][CH:11]([CH3:17])[C:12]([O:14][CH3:15])=[O:13]

参加物

5

反応物 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 18759635Ethyl 2-[2-({2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidine-1-yl]phenoxy}methyl)phenoxy]propionate

生成物 1

HCID 18759673Methyl 2-[2-({2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidine-1-yl]phenoxy}methyl)phenoxy]propionate収率 91.7%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Into 10 ml of methanol was dissolved 0.216 g of ethyl 2-[2-({2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidine-1-yl]phenoxy}methyl)phenoxy]propionate obtained in the above-described Production Example 3; a catalytic amount of sodium methoxide was added under ice-cooling and stirring and the mixture was stirred for 6 hours at room temperature. The reaction solution was poured into IN hydrochloric acid and the mixture was extracted twice with ethyl acetate. The organic layers were combined and washed once with a saturated aqueous sodium chloride solution, dried over magnesium sulfate and then concentrated under reduced pressure to give 0.193 g of methyl 2-[2-({ 2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidine-1-yl]phenoxy}methyl)phenoxy]propionate [Compound 3-1].

後処理

  1. customobtained in the above-described Production Example 3
  2. temperaturecooling
  3. stirringthe mixture was stirred for 6 hours at room temperature
  4. extractionthe mixture was extracted twice with ethyl acetate
  5. washwashed once with a saturated aqueous sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f9963eb998c94690a7da888384e34624
出典データセット
uspto-grants-2003_12
特許番号
US06664214B1

反応ノート

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