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Thionyl Chloride → 5-Chloro-4-chloromethyl-3-(4-chloro-phenyl)-1-phenyl-1H-pyrazole

HRID 441862
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HRID 441862 반응식
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[N:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:9]=[C:8]([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=2)[C:7]=1[CH2:24]O>C1C=CC=CC=1>[Cl:5][C:6]1[N:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:9]=[C:8]([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=2)[C:7]=1[CH2:24][Cl:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 53664379[5-Chloro-3-(4-chloro-phenyl)-1-phenyl-1H-pyrazol-4-yl]-methanol

생성물 1

HCID 540260095-Chloro-4-chloromethyl-3-(4-chloro-phenyl)-1-phenyl-1H-pyrazole수율 98.5%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

17.6 g of thionyl chloride are added to a suspension of 45 g of 5-chloro-3-p-chlorophenyl-4-hydroxymethyl-1-phenyl-pyrazole in 45 ml of benzene, there being a considerable evolution of gas and solution occurs. Following this heating is carried out for 30 minutes at boiling point for completion of the reaction. The solvent is distilled off in vacuo and this operation is carried out with the addition of benzene. The residue is caused to crystallise with the help of petroleum ether. 5-Chloro-4-chloromethyl-3-p-chlorophenyl-1-phenyl-pyrazole is obtained with a 98.5% yield; F 96.5°-97°.

후처리

  1. customfor completion of the reaction
  2. distillationThe solvent is distilled off in vacuo
  3. additionthis operation is carried out with the addition of benzene
  4. customto crystallise with the help of petroleum ether

출처 및 근거

ORD 기록
ord-7b2a46b886984b9887a6a7f3b04ffcae
출처 데이터셋
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04042702

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