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Hydrochloric Acid → HCID 59629257、化合物

HRID 1045302
ノート
印刷プレビュー

反応式

HRID 1045302 の反応式
Br[C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9](C4C=CC(C5C=CC6C(=CC=CC=6)C=5)=CC=4)=[CH:10][CH:11]=3)[CH:6]=[CH:5][C:4]=2[CH:3]=1.[CH3:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37].[CH2:38]([Li])[CH2:39][CH2:40][CH3:41].C([O:46][B:47](OC(C)C)[O:48]C(C)C)(C)C.Cl.[C:57]1(C)[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=1>C1COCC1>[CH:34]1[C:33]2[C:38](=[CH:39][CH:40]=[CH:41][CH:32]=2)[CH:37]=[CH:36][C:35]=1[C:57]1[CH:62]=[CH:61][C:60]([C:9]2[CH:8]=[C:7]3[C:12]([C:13]4[CH:14]=[CH:15][C:2]([B:47]([OH:48])[OH:46])=[CH:3][C:4]=4[CH:5]=[CH:6]3)=[CH:11][CH:10]=2)=[CH:59][CH:58]=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

8

反応物 6

HCID 313Hydrochloric AcidHCID 1140TolueneHCID 8058HexaneHCID 21531Triisopropyl borateHCID 59629116HCID 59629116、化合物HCID 178418339Butyllithium

生成物 1

HCID 59629257HCID 59629257、化合物収率 69%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

Under an argon gas atmosphere, a mixture of 15.0 g (32.7 mmol) of 2-bromo-7-(4-(naphthalene-2-yl)phenyl)phenanthrene and 150 mL of dehydrated THF was cooled down to minus 60 degree C. Then, 25.3 ml (39.2 mmol) of hexane solution of 1.55M n-butyllithium was dropped into the mixture while the mixture was being stirred. The reaction mixture was further stirred at minus 60 degrees for 2 hours. The reaction solution was again cooled down to minus 70 degrees C., and 18.4 g (98.0 mmol) of triisopropylborate was dropped into the solution. The reaction mixture was warmed back to room temperature, stirred for 2 hours and left unattended for one night. Subsequently, the reaction mixture was added with aqueous solution of hydrochloric acid while being cooled on an ice bath, and stirred for 1 hour at room temperature. The reaction mixture was added with toluene, and aqueous phase thereof was eliminated. After organic phase thereof was dried with magnesium sulfate, the solvent was distilled away under reduced pressure. By recrystallizing the obtained solid with toluene-hexane, 9.5 g of 7-(4-(naphthalene-2-yl)phenyl)phenanthrene-2-ylboronic acid was obtained at an yield of 69%.

後処理

  1. temperaturewas cooled down to minus 60 degree C
  2. stirringThe reaction mixture was further stirred at minus 60 degrees for 2 hours
  3. temperatureThe reaction mixture was warmed back to room temperature
  4. stirringstirred for 2 hours
  5. waitleft
  6. waitunattended for one night
  7. temperaturewhile being cooled on an ice bath
  8. stirringstirred for 1 hour at room temperature
  9. dry with materialAfter organic phase thereof was dried with magnesium sulfate
  10. distillationthe solvent was distilled away under reduced pressure
  11. customBy recrystallizing the obtained solid with toluene-hexane

出典と根拠

ORDレコード
ord-c33020058a2e468d84a3b264358029d5
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08568903B2

反応ノート

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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