1-chloro-2-fluoro-4-iodobenzene → 1-Chloro-2-fluoro-4-[(4-pentylphenyl)ethynyl]benzene

HRID 1613528ノート

反応式

HRID 1613528 の反応式
[CH2:1]([C:6]1[CH:11]=[CH:10][C:9]([C:12]#[CH:13])=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH2:4][CH3:5].[F:14][C:15]1[CH:16]=[C:17](I)[CH:18]=[CH:19][C:20]=1[Cl:21]>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I.C(NCC)C>[CH2:1]([C:6]1[CH:7]=[CH:8][C:9]([C:12]#[C:13][C:17]2[CH:18]=[CH:19][C:20]([Cl:21])=[C:15]([F:14])[CH:16]=2)=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH3:5]

参加物

6

反応物 2

HCID 27365631-chloro-2-fluoro-4-iodobenzeneHCID 27751311-Ethynyl-4-pentylbenzene

生成物 1

HCID 157452301-Chloro-2-fluoro-4-[(4-pentylphenyl)ethynyl]benzene

試薬・触媒・溶媒 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 178418476HCID 178418476、化合物触媒HCID 8021Diethylamine溶媒

実験手順

0.2 mmol of Pd(PPh3)2Cl2 and 0.1 mmol of CuI are added to a mixture of 0.01 mol of 4-pentylphenylacetylene, 0.01 mol of 3-fluoro-4-chloro-iodobenzene and 40 ml of diethylamine at room temperature and stirred for 12 hours. After completion of the reaction, the suspension is filtered, and the filtrate is concentrated by evaporation. Purification by chromatography and/or crystallization gives 4-pentyl-3'-fluoro-4'-chloro tolan having C 49.6° I.

後処理

  1. customAfter completion of the reaction
  2. filtrationthe suspension is filtered
  3. concentrationthe filtrate is concentrated by evaporation
  4. customPurification
  5. customby chromatography and/or crystallization

出典と根拠

ORDレコード
ord-27b81805cbca4584a94a315c6f563575
出典データセット
uspto-grants-1993_03
特許番号
US05194178

反応ノート

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