1-Chloro-4-isocyanato-2-(trifluoromethyl) benzene → HCID 57541570、化合物

HRID 1522920ノート

反応式

HRID 1522920 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].[NH2:15][C:16]1[CH:35]=[CH:34][C:19]([O:20][C:21]2[CH:26]=[CH:25][N:24]=[C:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH:22]=2)=[CH:18][CH:17]=1>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:10])[NH:15][C:16]2[CH:35]=[CH:34][C:19]([O:20][C:21]3[CH:26]=[CH:25][N:24]=[C:23]([C:27]([O:29][C:30]([CH3:31])([CH3:32])[CH3:33])=[O:28])[CH:22]=3)=[CH:18][CH:17]=2)=[CH:4][C:3]=1[C:11]([F:12])([F:13])[F:14]

参加物

4

反応物 2

HCID 27332651-Chloro-4-isocyanato-2-(trifluoromethyl) benzeneHCID 57541500HCID 57541500、化合物

生成物 1

HCID 57541570HCID 57541570、化合物収率 98.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

At room temperature, 1-chloro-4-isocyanato-2-(trifluoromethyl)benzene (656 mg, 2.96 mmol, 1.05 eq) was dissolved in dichloromethane (5 mL). To the resulted solution, a solution of tert-butyl 4-(4-aminophenoxy)picolinate (805 mg, 2.81 mmol, 1 eq) in dichloromethane (5 mL) was slowly added dropwise. The mixture was stirred for 16 hours at room temperature. The solvent was removed under reduced pressure, and the resulted solid was purified by column chromatography (dichloromethane:methanol=30:1) to give the title compound (1.4 g, purity 95%, yield 85%) as a white solid.

後処理

  1. customThe solvent was removed under reduced pressure
  2. customthe resulted solid was purified by column chromatography (dichloromethane:methanol=30:1)

出典と根拠

ORDレコード
ord-e2ff7a6926ce43afb2e22bad188d4f97
出典データセット
uspto-grants-2015_07
特許番号
US09078933B2

反応ノート

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