Thionyl Chloride → HCID 20485215, 화합물

HRID 647552노트

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HRID 647552 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 20485215HCID 20485215, 화합물수율 79%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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].

후처리

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

출처 및 근거

ORD 기록
ord-bf5089c6756942aba0314cc4ba5f91b0
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04409238

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