4-Methylphenylhydrazine monohydrochloride → 1-(4-Methylphenyl)pyrazolidin-3-one

HRID 133177

反応式

HRID 133177 の反応式
Cl.[C:2]1([CH3:10])[CH:7]=[CH:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1.C1CCN2C(=NCCC2)CC1.Br[CH2:23][CH2:24][C:25](Cl)=[O:26]>C(Cl)Cl>[CH3:10][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:23][CH2:24][C:25](=[O:26])[NH:9]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 125044-Methylphenylhydrazine monohydrochlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 84944Propanoyl chloride, 3-bromo-

生成物 1

HCID 19134851-(4-Methylphenyl)pyrazolidin-3-one収率 19,455.801%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

10 g of p-tolylhydrazine hydrochloride are dissolved in 100 ml of anhydrous CH2Cl2. The solution is cooled to 0° C. and 19 ml of DBU and then 6.5 mg of 3-bromopropionyl chloride are added. The mixture is stirred at ambient temperature for one hour. The reaction medium is poured onto water, extraction is carried out with CH2Cl2 and then purification is carried out by chromatography on a silica column eluted with an AcOEt/petroleum ether (v/v; 50/50) mixture. 1.3 g of crystals are obtained.

後処理

  1. additionThe reaction medium is poured onto water, extraction
  2. custompurification
  3. washeluted with an AcOEt/petroleum ether (v/v; 50/50) mixture

出典と根拠

ORDレコード
ord-e0d1fe6a07a74c78a3121edd965e5815
出典データセット
uspto-grants-2008_06
特許番号
US07390818B2

関連ノート

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