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

HRID 379691

反応式

HRID 379691 の反応式
[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

参加物

5

反応物 3

HCID 120252-PyrrolidoneHCID 24813Phosphorus oxychlorideHCID 766182-Cyclopropylaniline

生成物 1

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

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e5dfe8e4d0ab4a2594c4772221443df1
出典データセット
uspto-grants-2001_10
特許番号
US06300366B1

関連ノート

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