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

반응식

HRID 1978848 반응식
[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]

참가 물질

7

반응물 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

생성물 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

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매2회HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6ae1bdc470bb4dc3b04ffbb8d23cdc90
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06239074B1

연결된 노트

불러오는 중…