Water → 2,3-bis(4-fluorophenyl)-1-methyl-1H-pyrrole

HRID 1156313ノート

反応式

HRID 1156313 の反応式
[H-].[Na+].[F:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[NH:11][CH:12]=[CH:13][C:14]=2[C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)=[CH:6][CH:5]=1.[CH3:22]I.O>CS(C)=O>[F:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:11]([CH3:22])[CH:12]=[CH:13][C:14]=2[C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 111079192,3-bis(4-fluorophenyl)-1H-pyrrole

生成物 1

HCID 128733522,3-bis(4-fluorophenyl)-1-methyl-1H-pyrrole収率 79.8%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

実験手順

To a mixture of 1.5 g (0.038 mole) of 60% sodium hydride dispersion and 100 ml DMSO was added dropwise a solution of 5.1 g (0.02 mole) of 2,3-bis(4-fluorophenyl)-1H-pyrrole in 25 ml DMSO. After the mixture was stirred one hour at room temperature, 5.6 g (0.04 mole) of methyl iodide was added dropwise. The mixture was stirred at room temperature overnight, then poured into water and extracted with ether. The ether extracts were backwashed with water three times, then dried and concentrated. The crude solid was recrystallized from hexane to give 4.3 g of product, m.p. 129°-129.5°.

後処理

  1. stirringThe mixture was stirred at room temperature overnight
  2. extractionextracted with ether
  3. customdried
  4. concentrationconcentrated
  5. customThe crude solid was recrystallized from hexane

出典と根拠

ORDレコード
ord-00f35e09df13456d878e47f25e242bbd
出典データセット
uspto-grants-1982_06
特許番号
US04335136

反応ノート

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