Triethylamine → 4-{5-(2,4-dimethylbenzoyl)-1-methyl-1H-pyrrol-2-ylmethyl}nitrobenzene

HRID 365610

反応式

HRID 365610 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1.[CH3:17][C:18]1[CH:26]=[C:25]([CH3:27])[CH:24]=[CH:23][C:19]=1[C:20](Cl)=[O:21].C(N(CC)CC)C.[O-][Si]([O-])=O.[Mg+2]>CCCCCC.C(OCC)(=O)C.CCCCCC>[CH3:17][C:18]1[CH:26]=[C:25]([CH3:27])[CH:24]=[CH:23][C:19]=1[C:20]([C:6]1[N:2]([CH3:1])[C:3]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:5]=1)=[O:21]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 61680MAGNESIUM SILICATE (synthetic)HCID 1408672,4-Dimethylbenzoyl chlorideHCID 232857944-(1-Methylpyrrol-2-ylmethyl)nitrobenzene

生成物 1

HCID 232857664-{5-(2,4-dimethylbenzoyl)-1-methyl-1H-pyrrol-2-ylmethyl}nitrobenzene収率 42.3%

試薬・触媒・溶媒 2

HCID 8058Hexane溶媒HCID 21226206Ethyl acetate hexane溶媒

実験手順

4-(1-Methylpyrrol-2-ylmethyl)nitrobenzene (1.2 g, 5.5 mmol) [prepared as in Example 7, Step (b)], 2,4-dimethylbenzoyl chloride (1.6 g, 9.5 mmol), and triethylamine (1.3 ml, 9.3 mmol) were dissolved in xylenes (50 ml), and the reaction mixture was heated at reflux under argon. After 48 h, the reaction mixture was passed through a Florisil® column (hexane followed by hexane-ethyl acetate, 95:5) to give 4-{5-(2,4-dimethylbenzoyl)-1-methyl-1H-pyrrol-2-yl-methyl}nitrobenzene (0.81 g, 42%) as a solid. ##STR40##

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux under argon

出典と根拠

ORDレコード
ord-93d1aaf0ca7f4f31a6b2479a02a6d63a
出典データセット
uspto-grants-2000_10
特許番号
US06127402

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