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Hydrochloric Acid → 9,9-dimethyl-7-(naphthalene-2-yl)-9H-fluorene-2-ylboronic acid

HRID 1429319
ノート
印刷プレビュー

反応式

HRID 1429319 の反応式
Br[C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8](C4C=CC5C(=CC=CC=5)C=4)=[CH:9][CH:10]=3)[C:5]([CH3:26])([CH3:25])[C:4]=2[CH:3]=1.[CH2:27]([Li])[CH2:28][CH2:29][CH3:30].[B:32](OC(C)C)([O:37]C(C)C)[O:33]C(C)C.Cl.[CH3:46][CH2:47][CH2:48][CH2:49][CH2:50][CH3:51]>ClCCl.C1COCC1>[CH3:26][C:5]1([CH3:25])[C:6]2[CH:7]=[C:8]([B:32]([OH:37])[OH:33])[CH:9]=[CH:10][C:11]=2[C:12]2[C:4]1=[CH:3][C:2]([C:48]1[CH:47]=[CH:46][C:30]3[C:50](=[CH:51][CH:27]=[CH:28][CH:29]=3)[CH:49]=1)=[CH:14][CH:13]=2
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 5

HCID 313Hydrochloric AcidHCID 8058HexaneHCID 21531Triisopropyl borateHCID 576228742-bromo-9,9-dimethyl-7-(naphthalene-2-yl)-9H-fluoreneHCID 178418339Butyllithium

生成物 1

HCID 674212339,9-dimethyl-7-(naphthalene-2-yl)-9H-fluorene-2-ylboronic acid収率 64%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-60 °C

実験手順

In argon atmosphere, a liquid mixture of 6.00 g (15.0 mmol) of 2-bromo-9,9-dimethyl-7-(naphthalene-2-yl)-9H-fluorene and 150 ml of dry THF was cooled to −60° C., and 11.6 ml (18.0 mmol) of a 1.55 M hexane solution of n-butyllithium was added dropwise under stirring. Then, the reaction mixture was stirred at −70° C. for 2 h. The reaction solution was cooled again to −70° C., and 8.48 g (45.1 mol) of triisopropyl borate was added dropwise. The reaction mixture was heated up to room temperature, stirred for one hour, and left standing overnight. The reaction mixture was cooled on ice bath, added with a 6 N hydrochloric acid, and stirred at room temperature for one hour. The reaction mixture was added with dichloromethane and allowed to stand for separation into liquid phases. The organic phase was washed with water and dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel chromatography to obtain 3.50 g (yield: 64%) of 9,9-dimethyl-7-(naphthalene-2-yl)-9H-fluorene-2-ylboronic acid.

後処理

  1. stirringThen, the reaction mixture was stirred at −70° C. for 2 h
  2. temperatureThe reaction solution was cooled again to −70° C.
  3. temperatureThe reaction mixture was heated up to room temperature
  4. stirringstirred for one hour
  5. waitleft
  6. temperatureThe reaction mixture was cooled on ice bath
  7. stirringstirred at room temperature for one hour
  8. customto stand for separation into liquid phases
  9. washThe organic phase was washed with water
  10. dry with materialdried over sodium sulfate
  11. distillationThe solvent was distilled off under reduced pressure
  12. customthe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-bce3815598664c389676f27fd1fbf3a3
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08940412B2

反応ノート

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