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

HRID 511757ノート

反応式

HRID 511757 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-529e588ce9ac4b44a6f63472709bc656
出典データセット
uspto-grants-2015_08
特許番号
US09101135B2

反応ノート

読み込み中…