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Water → HCID 58836110、化合物

HRID 600155
ノート
印刷プレビュー

反応式

HRID 600155 の反応式
Br[C:2]1[C:3]2[C:8]([C:9]([C:16]3[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=3)=[C:10]3[C:15]=1[CH:14]=[CH:13][CH:12]=[CH:11]3)=[CH:7][CH:6]=[CH:5][CH:4]=2.[Li]CCCC.C(O[B:32]1[O:36][C:35]([CH3:38])([CH3:37])[C:34]([CH3:40])([CH3:39])[O:33]1)(C)C.O>C1COCC1>[CH3:39][C:34]1([CH3:40])[C:35]([CH3:38])([CH3:37])[O:36][B:32]([C:2]2[C:3]3[C:8]([C:9]([C:16]4[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=4)=[C:10]4[C:15]=2[CH:14]=[CH:13][CH:12]=[CH:11]4)=[CH:7][CH:6]=[CH:5][CH:4]=3)[O:33]1
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

6

反応物 4

HCID 962WaterHCID 50177412-Isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolaneHCID 14934743HCID 14934743、化合物HCID 178418339Butyllithium

生成物 1

HCID 58836110HCID 58836110、化合物収率 67%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

4.6 g (1 eq, 13.25 mmol) of 9-bromo-10-p-tolyl-anthracene was dissolved in 150 ml of THF in a 500 ml round-bottomed flask in Ar gas condition, and 6.36 ml (1.2 eq, 15.9 mmol) of 2.5M n-BuLi (in hexane) was added to the solution at −78° C. After stirring the solution at −78° C. for 1 hour, 3.52 ml (1.3 eq, 17.23 mmol) of 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane was added to the solution and stirred at room temperature for 2 hours. Next, 50 ml of water was added to the solution to terminate the reaction, and the organic phase of the solution was extracted using brine and methylene chloride. The extracted organic phase was dried using anhydrous magnesium sulfate and filtered to remove the solvent. The dried organic phase was dissolved in a small amount of toluene and subjected to column chromatography (silica and hexane) to remove impurities. Next, the polarity of the eluent solvent was increased to obtain 3.5 g (67%) of a white solid.

後処理

  1. additionwas added to the solution at −78° C
  2. stirringstirred at room temperature for 2 hours
  3. customto terminate
  4. customthe reaction
  5. extractionthe organic phase of the solution was extracted
  6. customThe extracted organic phase was dried
  7. filtrationfiltered
  8. customto remove the solvent
  9. dissolutionThe dried organic phase was dissolved in a small amount of toluene
  10. customto remove impurities
  11. temperatureNext, the polarity of the eluent solvent was increased

出典と根拠

ORDレコード
ord-f4db59bbd2d0419f81a89a2b3bf28b4f
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07901793B2

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