N-Methylisopropylamine → 3-[4-Chloro-2-fluoro-5-{[isopropyl(methyl)amino]carbonylaminosulfonyl}phenyl]-1-methyl-2,4-dioxo-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

HRID 18678

反応式

HRID 18678 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[N:11]([CH3:20])[C:10]2=[O:21])=[CH:4][C:3]=1[S:22]([N:25]=[C:26]=[O:27])(=[O:24])=[O:23].[CH3:28][NH:29][CH:30]([CH3:32])[CH3:31]>ClCCCl>[Cl:1][C:2]1[C:3]([S:22]([NH:25][C:26]([N:29]([CH:30]([CH3:32])[CH3:31])[CH3:28])=[O:27])(=[O:24])=[O:23])=[CH:4][C:5]([N:9]2[C:14](=[O:15])[CH:13]=[C:12]([C:16]([F:19])([F:17])[F:18])[N:11]([CH3:20])[C:10]2=[O:21])=[C:6]([F:8])[CH:7]=1

参加物

4

反応物 2

HCID 78485N-MethylisopropylamineHCID 587094392-Chloro-4-fluoro-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-trifluoromethyl-(2H)-pyrimidin-1-yl]benzenesulfonylisocyanate

生成物 1

HCID 587094373-[4-Chloro-2-fluoro-5-{[isopropyl(methyl)amino]carbonylaminosulfonyl}phenyl]-1-methyl-2,4-dioxo-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒2 回

実験手順

With stirring, 1.0 g (2.34 mmol) of 2-chloro-4-fluoro-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-trifluoromethyl-(2H)-pyrimidin-1-yl]benzenesulfonyl isocyanate in 1,2-dichloroethane was added to a solution of 0.34 g (4.68 mmol) of N-methylisopropylamine in 1,2-dichloroethane, and the mixture was stirred overnight. The reaction mixture was concentrated, the residue was taken up in methylene chloride and 0.5N hydrochloric acid was added. The organic phase was then dried and the solvent was removed. This gave 0.5 g (42% of theory) of the title compound as a colorless solid (m.p.: 145° C.).

後処理

  1. stirringthe mixture was stirred overnight
  2. concentrationThe reaction mixture was concentrated
  3. addition0.5N hydrochloric acid was added
  4. customThe organic phase was then dried
  5. customthe solvent was removed

出典と根拠

ORDレコード
ord-dfb6cfc1a7aa40f98611b46339d471c2
出典データセット
uspto-grants-2010_06
特許番号
US07741485B2

関連ノート

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