Pyridine → 2,6-Dimethyl-4-(nonafluoro-2-butyl)phenyl 3-[(2,2,2-trichloroethoxy)carbonylamino]benzamide

HRID 511757노트

반응식

HRID 511757 반응식
[CH3:1][C:2]1[CH:8]=[C:7]([C:9]([F:21])([C:14]([F:20])([F:19])[C:15]([F:18])([F:17])[F:16])[C:10]([F:13])([F:12])[F:11])[CH:6]=[C:5]([CH3:22])[C:3]=1N.[N:23]1C=CC=CC=1.O1CCCC1.[Cl:34][C:35]([Cl:51])([Cl:50])[CH2:36][O:37][C:38]([NH:40][C:41]1[CH:42]=[C:43]([CH:47]=[CH:48][CH:49]=1)[C:44](Cl)=[O:45])=[O:39]>O.C(OCC)(=O)C>[CH3:22][C:5]1[CH:6]=[C:7]([C:9]([F:21])([C:14]([F:19])([F:20])[C:15]([F:16])([F:17])[F:18])[C:10]([F:11])([F:12])[F:13])[CH:8]=[C:2]([CH3:1])[C:3]=1[C:42]1[C:41]([NH:40][C:38]([O:37][CH2:36][C:35]([Cl:51])([Cl:50])[Cl:34])=[O:39])=[CH:49][CH:48]=[CH:47][C:43]=1[C:44]([NH2:23])=[O:45]

참가 물질

7

반응물 4

HCID 1049PyridineHCID 8028TetrahydrofuranHCID 231237403-[(2,2,2-Trichloroethoxy)carbonylamino]benzoyl chlorideHCID 866700812,6-Dimethyl-4-(nonafluoro-2-butyl)aniline

생성물 1

HCID 866700802,6-Dimethyl-4-(nonafluoro-2-butyl)phenyl 3-[(2,2,2-trichloroethoxy)carbonylamino]benzamide수율 71.2%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

First, to a solution prepared by adding 0.34 g of 2,6-dimethyl-4-(nonafluoro-2-butyl)aniline and 0.09 g of pyridine to 5 ml of tetrahydrofuran and stirring the resultant mixture at room temperature was added 0.33 g of 3-[(2,2,2-trichloroethoxy)carbonylamino]benzoyl chloride produced in Example 9-2. After reaction for 5 hours, ethyl acetate and water were added to the reaction solution, and a separating operation was performed. Then, an organic layer was separated and dried with anhydrous magnesium sulfate. The solution was filtered, and then the filtrate was collected, and the solvent of the filtrate was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate=4:1) to obtain 0.45 g (yield 71%) of the title compound as a solid.

후처리

  1. customFirst, to a solution prepared
  2. customAfter reaction for 5 hours
  3. customThen, an organic layer was separated
  4. dry with materialdried with anhydrous magnesium sulfate
  5. filtrationThe solution was filtered
  6. customthe filtrate was collected
  7. distillationthe solvent of the filtrate was distilled off under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-529e588ce9ac4b44a6f63472709bc656
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09101135B2

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