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Water → HCID 178447940、化合物

HRID 857591
ノート
印刷プレビュー

反応式

HRID 857591 の反応式
FC(F)(F)S(O[C:7]1[CH:16]=[CH:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([C:17]3[CH:22]=[C:21]([F:23])[C:20]([F:24])=[C:19]([F:25])[CH:18]=3)[CH:13]=2)C=1)(=O)=O.[C:28]([CH:30]1[CH2:35][CH2:34][CH:33]([CH2:36][CH2:37][CH3:38])[CH2:32][CH2:31]1)#[CH:29].O.[CH3:40]N(C)C=O>C(N(CC)CC)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[Cu](I)I>[CH2:28]([C@H:30]1[CH2:35][CH2:34][C@H:33]([C:36]#[C:37][C:38]2[C:9]3[C:14](=[CH:13][C:12]([C:17]4[CH:18]=[C:19]([F:25])[C:20]([F:24])=[C:21]([F:23])[CH:22]=4)=[CH:11][CH:10]=3)[CH:15]=[CH:16][CH:7]=2)[CH2:32][CH2:31]1)[CH2:29][CH3:40]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 218700436-(3,4,5-Trifluorophenyl)naphthalene-2-yl trifluoromethanesulfonateHCID 218706261-Ethynyl-4-propylcyclohexane

生成物 1

HCID 178447940HCID 178447940、化合物

試薬・触媒・溶媒 3

HCID 83717Copper iodide触媒
HCID 178418397HCID 178418397、化合物触媒
HCID 8471Triethylamine溶媒

反応条件

温度
50 °C

実験手順

25.0 g of 6-(3,4,5-trifluorophenyl)naphthalene-2-yl trifluoromethanesulfonate and 1-ethynyl-4-propylcyclohexane were dissolved in a mixture of 125 ml of N,N-dimethylformamide and 25 ml of triethylamine. To the solution were then added 0.7 g of tetrakis(triphenylphosphine)palladium and 0.2 g of copper iodide (I). The reaction mixture was then stirred at a temperature of 50° C. for 3 hours. The reaction solution was then allowed to cool to room temperature. To the reaction solution was then added 150 ml of water. The reaction solution was extracted with 200 ml of toluene, washed with water and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was then distilled off. The residue was then recrystallized from ethanol to obtain 17.6 g of 2-(trans-4-propylcyclohexyl)ethynyl-6-(3,4,5-trifluorophenyl)naphthalene.

後処理

  1. temperatureto cool to room temperature
  2. extractionThe reaction solution was extracted with 200 ml of toluene
  3. washwashed with water and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was then distilled off
  6. customThe residue was then recrystallized from ethanol

出典と根拠

ORDレコード
ord-8ab84d3100a24c7a85ae7395431a3675
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07145047B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート