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

HRID 441862
ノート
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反応式

HRID 441862 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-7b2a46b886984b9887a6a7f3b04ffcae
出典データセット
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04042702

反応ノート

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