Sodium Carbonate → HCID 59229504、化合物

HRID 1640097

反応式

HRID 1640097 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11])[CH2:5]Cl.[F:13][C:14]([F:29])([F:28])[C:15]1[CH:16]=[C:17](B(O)O)[CH:18]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:20]=1.C(=O)([O-])[O-].[Na+].[Na+]>O.COCCOC.C(OCC)(=O)C>[F:13][C:14]([F:28])([F:29])[C:15]1[CH:16]=[C:17]([CH:18]=[C:19]([C:21]([F:22])([F:23])[F:24])[CH:20]=1)[CH2:5][C:4]1[CH:7]=[CH:8][C:9]([N+:10]([O-:12])=[O:11])=[C:2]([CH3:1])[CH:3]=1

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 87687Alpha-chloro-3-methyl-4-nitrotolueneHCID 1562653,5-Bis-trifluoromethylphenylboronic acid

生成物 1

HCID 59229504HCID 59229504、化合物収率 83.3%

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 80711,2-Dimethoxyethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 3-methyl-4-nitrobenzyl chloride (0.27 g), 3,5-bis-(trifluoromethyl)phenylboronic acid (0.45 g), tetrakis(triphenylphosfine)palladium (0.1 g) and sodium carbonate (0.48 g) in water (2 ml) and 1,2-dimethoxyethane (10 ml) was stirred under an argon atmosphere at 85° C. for 2 hours. After cooling, the reaction solution was diluted with ethyl acetate and further stirred for 10 minutes by adding water thereto. After washing the organic layer with a saturated salt solution, it was dried over anhydrous magnesium sulfate. The solution was distilled off under reduced pressure and the resultant residue was purified by silica gel column chromatography to obtain 4-(3,5-bis-trifluoromethyl-benzyl)-2-methyl-nitrobenzene (0.44 g).

後処理

  1. temperatureAfter cooling
  2. washAfter washing the organic layer with a saturated salt solution, it
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. distillationThe solution was distilled off under reduced pressure
  5. customthe resultant residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-8c6e98deb47f4c6d8b0369cd3fdafd97
出典データセット
uspto-grants-2012_02
特許番号
US08110689B2

関連ノート

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