Water → 3-[4-Chloro-3-(2-(2,2,2-trifluoroethoxycarbonyl)-ethenyl)-phenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

HRID 1978848

反応式

HRID 1978848 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[N:10]([CH3:19])[C:9]2=[O:20])=[CH:4][C:3]=1I.[C:22]([O:26][CH2:27][C:28]([F:31])([F:30])[F:29])(=[O:25])[CH:23]=[CH2:24].C([O-])(=O)C.[Na+].O>CN(C)C=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH:12]=[C:11]([C:15]([F:18])([F:17])[F:16])[N:10]([CH3:19])[C:9]2=[O:20])=[CH:4][C:3]=1[CH:24]=[CH:23][C:22]([O:26][CH2:27][C:28]([F:31])([F:30])[F:29])=[O:25]

参加物

7

反応物 4

HCID 962WaterHCID 678892,2,2-Trifluoroethyl acrylateHCID 517045Sodium AcetateHCID 212012343-[4-Chloro-3-iodophenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

生成物 1

HCID 865837943-[4-Chloro-3-(2-(2,2,2-trifluoroethoxycarbonyl)-ethenyl)-phenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒2 回HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

A suspension of 5.0 g of 3-[4-chloro-3-iodophenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine, 2.0 g of 2,2,2-trifluoroethyl acrylate, 0.5 mg of palladium acetate and 1.1 g of sodium acetate in 50 ml of dimethylformamide was stirred for 4 hours at 120° C., after which further palladium acetate and 2,2,2-trifluoromethyl acrylate were added and stirring was continued for a further 2 hours at 120° C. The cooled reaction mixture was added to 200 ml of water and the precipitate was isolated, washed with petroleum ether and dried under greatly reduced pressure.

後処理

  1. stirringstirring
  2. waitwas continued for a further 2 hours at 120° C
  3. customThe cooled reaction mixture
  4. customthe precipitate was isolated
  5. washwashed with petroleum ether
  6. customdried under greatly reduced pressure

出典と根拠

ORDレコード
ord-6ae1bdc470bb4dc3b04ffbb8d23cdc90
出典データセット
uspto-grants-2001_05
特許番号
US06239074B1

関連ノート

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