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Hydrochloric Acid → 5-Chloro-4-chloromethyl-3-(4-chloro-phenyl)-1-phenyl-1H-pyrazole

HRID 441863
ノート
印刷プレビュー

反応式

HRID 441863 の反応式
[ClH:1].[Cl:2][C:3]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:6]=[C:5]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[C:4]=1[CH2:21]O>C1(C)C=CC=CC=1>[Cl:2][C:3]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:6]=[C:5]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[C:4]=1[CH2:21][Cl:1]
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 313Hydrochloric Acid2 回HCID 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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Hydrogen chloride gas is introduced into a mixture of 15 g of 5-chloro-3-p-chlorophenyl-4-hydroxymethyl-1-phenylpyrazole and 25 ml of concentrated hydrochloric acid and heating is carried out for 4 hours at boiling point. Following this 25 ml of toluene are mixed in. The layers are separated and the aqueous phase with toluene is removed. The organic layers are reduced in bulk by evaporation in vacuo, toluene is again added and reduction in bulk is repeated. 5-Chloro-4-chloromethyl-3-p-chlorophenyl-1-phenyl-pyrazole is obtained with a quantitative yield; F 96.5°-97° (from petroleum ether).

後処理

  1. temperatureheating
  2. additionare mixed in
  3. customThe layers are separated
  4. customthe aqueous phase with toluene is removed
  5. customThe organic layers are reduced in bulk by evaporation in vacuo, toluene
  6. additionis again added

出典と根拠

ORDレコード
ord-fb8e36b3867845e98cdf966d99d0f169
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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