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

HRID 133177

반응식

HRID 133177 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e0d1fe6a07a74c78a3121edd965e5815
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390818B2

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