1-Chloro-4-isocyanato-2-(trifluoromethyl) benzene → HCID 57541570, 화합물

HRID 1184942노트

반응식

HRID 1184942 반응식
[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]

참가 물질

4

반응물 2

HCID 27332651-Chloro-4-isocyanato-2-(trifluoromethyl) benzeneHCID 57541500HCID 57541500, 화합물

생성물 1

HCID 57541570HCID 57541570, 화합물수율 98.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

At room temperature, 1-chloro-4-isocyanato-2-(trifluoromethyl)benzene (656 mg, 2.96 mmol, 1.05 eq) was disolved 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 (dichoromethane:methanol=30:1) to give the title compound (1.4 g, putity 95%, yield 85%) as a white solid.

후처리

  1. customAt room temperature
  2. customThe solvent was removed under reduced pressure
  3. customthe resulted solid was purified by column chromatography (dichoromethane:methanol=30:1)

출처 및 근거

ORD 기록
ord-564417a45fc347889dc003874766d554
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08669369B2

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