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1-Chloro-4-isocyanato-2-(trifluoromethyl) benzene → 1-(4-Chloro-3-trifluoromethyl-phenyl)-3-[2-chloro-4-(2-methylsulfanyl-pyrimidin-4-yloxy)-phenyl]-urea

HRID 659014
ノート
印刷プレビュー

反応式

HRID 659014 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[O:10])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].[Cl:15][C:16]1[CH:21]=[C:20]([O:22][C:23]2[CH:28]=[CH:27][N:26]=[C:25]([S:29][CH3:30])[N:24]=2)[CH:19]=[CH:18][C:17]=1[NH2:31]>C1COCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:31][C:17]2[CH:18]=[CH:19][C:20]([O:22][C:23]3[CH:28]=[CH:27][N:26]=[C:25]([S:29][CH3:30])[N:24]=3)=[CH:21][C:16]=2[Cl:15])=[O:10])=[CH:4][C:3]=1[C:11]([F:12])([F:13])[F:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 27332651-Chloro-4-isocyanato-2-(trifluoromethyl) benzeneHCID 675239652-Chloro-4-(2-methylsulfanyl-pyrimidin-4-yloxy)-phenylamine

生成物 1

HCID 675240581-(4-Chloro-3-trifluoromethyl-phenyl)-3-[2-chloro-4-(2-methylsulfanyl-pyrimidin-4-yloxy)-phenyl]-urea収率 26.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 281 mg (1.27 mmol) 4-chloro-3-trifluoromethyl-phenyl isocyanate in 3 ml THF was added within 5 min. drop by drop at 0° C. to a solution of 340 mg (1.27 mmol) 2-chloro-4-(2-methylsulfanyl-pyrimidin-4-yloxy)-phenylamine and stirring continued at r.t. overnight. The reaction mixture was evaporated and purified by chromatography on silica (ethyl acetate/isohexane 1:4) to give 162 mg (26%) 1-(4-chloro-3-trifluoromethyl-phenyl)-3-[2-chloro-4-(2-methylsulfanyl-pyrimidin-4-yloxy)-phenyl]-urea.

後処理

  1. customThe reaction mixture was evaporated
  2. custompurified by chromatography on silica (ethyl acetate/isohexane 1:4)

出典と根拠

ORDレコード
ord-5cfba7548b144640be00cc64810b95b4
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08080552B2

反応ノート

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