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

HRID 1429319
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HRID 1429319 반응식
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
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참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

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온도
-60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bce3815598664c389676f27fd1fbf3a3
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08940412B2

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