2-Pyrrolidone → N-(2-Cyclopropylphenyl)-3,4-dihydro-2H-pyrrol-5-amine hydrochloride

HRID 379691

반응식

HRID 379691 반응식
[NH:1]1[CH2:5][CH2:4][CH2:3][C:2]1=O.P(Cl)(Cl)([Cl:9])=O.[CH:12]1([C:15]2[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=2[NH2:17])[CH2:14][CH2:13]1>ClCCCl>[ClH:9].[CH:12]1([C:15]2[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=2[NH:17][C:2]2[CH2:3][CH2:4][CH2:5][N:1]=2)[CH2:14][CH2:13]1

참가 물질

5

반응물 3

HCID 120252-PyrrolidoneHCID 24813Phosphorus oxychlorideHCID 766182-Cyclopropylaniline

생성물 1

HCID 18368246N-(2-Cyclopropylphenyl)-3,4-dihydro-2H-pyrrol-5-amine hydrochloride

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
60 °C

실험 절차

5 mmol (425 mg) of 2-pyrrolidinone and 5 mmol (766 mg) of phosphorus oxychloride are added to a solution of 5 mmol (666 mg) of 2-cyclopropylaniline in 30 ml of 1,2-dichloroethane. The whole is heated at 60° C. for 3.5 hours. After evaporation of the solvent, the residue is taken up in water, rendered alkaline with the aid of sodium carbonate, and extracted twice with 100 ml of ether. The organic phase is then dried, concentrated and purified by chromatography on silica gel to yield the expected product. The corresponding hydrochloride is obtained by the action of a titrated solution of hydrochloric acid in ethanol.

후처리

  1. customAfter evaporation of the solvent
  2. extractionextracted twice with 100 ml of ether
  3. customThe organic phase is then dried
  4. concentrationconcentrated
  5. custompurified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-e5dfe8e4d0ab4a2594c4772221443df1
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300366B1

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