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

HRID 1156313노트

반응식

HRID 1156313 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-00f35e09df13456d878e47f25e242bbd
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04335136

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