Thionyl Chloride → HCID 20485215、化合物

HRID 647552ノート

反応式

HRID 647552 の反応式
[Cl:1][C:2]([Cl:12])=[CH:3][CH2:4][CH:5]([CH:9]([CH3:11])[CH3:10])[C:6](O)=[O:7].S(Cl)([Cl:15])=O>C1C=CC=CC=1>[Cl:1][C:2]([Cl:12])=[CH:3][CH2:4][CH:5]([CH:9]([CH3:11])[CH3:10])[C:6]([Cl:15])=[O:7]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 129596915,5-Dichloro-2-isopropyl-4-pentenoic acid

生成物 1

HCID 20485215HCID 20485215、化合物収率 79%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To 2.1 g of α-(3,3-dichloroallyl)isovaleric acid were added 3.0 g of thionyl chloride, as well as 10 g of benzene, and the mixture was refluxed for 5 hours. Then, the reaction mixture was distilled to remove the low-boiling fraction. By this procedure there was obtained α-(3,3-dichloroallyl)isovaleroyl chloride. This chloride was dissolved in 30 g of dry benzene, followed by the addition of 2.0 g of 3-phenoxybenzyl alcohol. Then, 2.0 g of pyridine were added added dropwise and the mixture was stirred at room temperature overnight. The reaction mixture was then diluted with diethyl ether, washed with dilute hydrochloric acid and water, dried over anhydrous magnesium sulfate and distilled to remove the low-boiling fraction. The residual viscous oil was purified by column chromatography to recover 3.1 g of 3-phenoxybenzyl α-(3,3-dichloroallyl)isovalerate (Compound [5]) having the following properties [yield: 79% based on α-(3,3-dichloroallyl)isovaleric acid].

後処理

  1. distillationThen, the reaction mixture was distilled
  2. customto remove the low-boiling fraction

出典と根拠

ORDレコード
ord-bf5089c6756942aba0314cc4ba5f91b0
出典データセット
uspto-grants-1983_10
特許番号
US04409238

反応ノート

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