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(3-Bromo-4-fluorophenoxy)(tert-butyl)dimethylsilane → 5-Dimethylaminomethyl-6-(2-fluoro-5-hydroxy-phenyl)-spiro[2.5]octan-6-ol

HRID 2404608
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인쇄 미리보기

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HRID 2404608 반응식
Br[C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[F:16])[O:5][Si](C(C)(C)C)(C)C.[Li]CCCC.[CH3:22][N:23]([CH2:25][CH:26]1[C:33](=[O:34])[CH2:32][CH2:31][C:28]2([CH2:30][CH2:29]2)[CH2:27]1)[CH3:24]>C1COCC1.CCCCCC>[CH3:24][N:23]([CH2:25][CH:26]1[C:33]([C:2]2[CH:3]=[C:4]([OH:5])[CH:13]=[CH:14][C:15]=2[F:16])([OH:34])[CH2:32][CH2:31][C:28]2([CH2:30][CH2:29]2)[CH2:27]1)[CH3:22]
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참가 물질

6

반응물 3

HCID 59315494(3-Bromo-4-fluorophenoxy)(tert-butyl)dimethylsilaneHCID 682910585-Dimethylaminomethyl-spiro[2.5]octan-6-oneHCID 178418339Butyllithium

생성물 1

HCID 601424765-Dimethylaminomethyl-6-(2-fluoro-5-hydroxy-phenyl)-spiro[2.5]octan-6-ol수율 36.3%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회
HCID 8058
Hexane
용매

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온도
-78 °C

실험 절차

Cool a solution of (3-bromo-4-fluoro-phenoxy)-tert-butyl-dimethyl-silane (472 mg, 1.547 mmol) in THF (40 mL) to −78° C. under N2. Then add dropwise a solution of n-BuLi (0.63 mL, 1.547 mmol) in hexane via syringe to the reaction solution. After being stirred at −78° C. for 2 hour, add dropwise a solution of 5-Dimethylaminomethyl-spiro[2.5]octan-6-one (70 mg, 0.387 mmol) in THF (1 mL) to the reaction mixture and stir the mixture at −78° C. for additional 2 hours. Quench the reaction with 20 mL of diluted HCl (2N), and stir at ambient temperature for 2 hours. Basify the resultant mixture with K2CO3 to pH=9, and extract with EtOAc (30 mL×2). The combined organic layers are washed with brine, dried over Na2SO4, filtered, and concentrated under vacuum. Purify the residue by silica gel chromatography (CH2Cl2 to CH2Cl2:MeOH=10:1) to afford 5-dimethylaminomethyl-6-(2-fluoro-5-hydroxy-phenyl)-spiro[2.5]octan-6-ol as white solid (41 mg, yield: 36.3%). MS (m/z): 294 (M+1).

후처리

  1. stirringstir the mixture at −78° C. for additional 2 hours
  2. customQuench
  3. customthe reaction with 20 mL of diluted HCl (2N)
  4. stirringstir at ambient temperature for 2 hours
  5. extractionBasify the resultant mixture with K2CO3 to pH=9, and extract with EtOAc (30 mL×2)
  6. washThe combined organic layers are washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum
  10. customPurify the residue by silica gel chromatography (CH2Cl2 to CH2Cl2:MeOH=10:1)

출처 및 근거

ORD 기록
ord-63d4f0061245490fa7b06819f3082945
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08802728B2

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