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Magnesium → HCID 22141592、化合物

HRID 270243
ノート
印刷プレビュー

反応式

HRID 270243 の反応式
Br[C:2]1[S:3][CH:4]=[CH:5][C:6]=1[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[Mg].Br[C:17]1[S:21][C:20]([C:22]2[CH:27]=[C:26]([O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[C:25]([C:37]3[S:38][C:39](Br)=[CH:40][CH:41]=3)=[CH:24][C:23]=2[O:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH3:51])=[CH:19][CH:18]=1>C1COCC1.C(OCC)(=O)C>[CH2:7]([C:6]1[CH:5]=[CH:4][S:3][C:2]=1[C:17]1[S:21][C:20]([C:22]2[CH:27]=[C:26]([O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[C:25]([C:37]3[S:38][C:39]([C:2]4[S:3][CH:4]=[CH:5][C:6]=4[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])=[CH:40][CH:41]=3)=[CH:24][C:23]=2[O:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH3:51])=[CH:19][CH:18]=1)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 5462224MagnesiumHCID 107548542-Bromo-3-n-octylthiopheneHCID 221415882,2'-[2,5-Bis(octyloxy)-1,4-phenylene]bis(5-bromothiophene)

生成物 1

HCID 22141592HCID 22141592、化合物収率 30%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒3 回
HCID 8857
Ethyl Acetate
溶媒

実験手順

A solution of 2-bromo-3-octylthiophene (1.800 grams, 6.533 mmol) in 7 milliliters of anhydrous THF was added slowly over a period of 20 minutes to a mechanically stirred suspension of magnesium turnings (0.238 grams, 9.79 mmol) in 3 milliliters of THF in a 250 milliliter round-bottomed flask under an inert argon atmosphere. The resultant mixture was stirred at 60° C. for 4 hours, and then cooled down to room temperature. The resultant mixture was then added via a cannula to a mixture of 1,4-bis(5-bromo-2-thienyl)-2,5-dioctyloxybenzene (1.650 grams, 2.513 mmol) and [1,3-bis(diphenylphosphinopropane]dichloronickel (II) (0.057 gram, 0.105 mmol) in 20 milliliters of anhydrous THF in a 250 milliliter round-bottomed flask under an inert atmosphere, and refluxed for 48 hours. Subsequently, the reaction mixture was diluted with 200 milliliters of ethyl acetate, was washed twice with water and dried with anhydrous magnesium sulfate. A brown solid, obtained after evaporation of the solvent, was purified by column chromotography on silica gel and recrystallized yielding 1,4-bis[5-(3-octyl-2-thienyl)-2-thienyl]-2,5-dioctyloxybenzene as a yellow crystalline product in 30 percent yield.

後処理

  1. washwas washed twice with water
  2. dry with materialdried with anhydrous magnesium sulfate
  3. customA brown solid, obtained
  4. customafter evaporation of the solvent
  5. customwas purified by column chromotography on silica gel
  6. customrecrystallized

出典と根拠

ORDレコード
ord-aa80b1f9b2384a9789906b671317bbca
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07449542B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート