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

HRID 365610

반응식

HRID 365610 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 8058Hexane용매HCID 21226206Ethyl acetate hexane용매

실험 절차

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##

후처리

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

출처 및 근거

ORD 기록
ord-93d1aaf0ca7f4f31a6b2479a02a6d63a
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127402

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