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Benzyl Alcohol → 2-(Benzyloxy)-3-bromobenzonitrile

HRID 1497948
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HRID 1497948 반응식
[H-].[Na+].[CH2:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Br:11][C:12]1[C:13](F)=[C:14]([CH:17]=[CH:18][CH:19]=1)[C:15]#[N:16]>CN(C=O)C>[CH2:3]([O:10][C:13]1[C:12]([Br:11])=[CH:19][CH:18]=[CH:17][C:14]=1[C:15]#[N:16])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
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참가 물질

5

반응물 3

HCID 244Benzyl AlcoholHCID 24758Sodium hydrideHCID 27612003-Bromo-2-fluorobenzonitrile

생성물 1

HCID 598089582-(Benzyloxy)-3-bromobenzonitrile수율 71.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
0 °C

실험 절차

To a flask containing sodium hydride (1.44 g, 60.0 mmol) suspended in DMF (60 mL, 800 mmol) at 0° C. was added benzyl alcohol (6.21 mL, 60.0 mmol) over 5 min. The reaction mixture was stirred at 0° C. for 30 min and then 3-bromo-2-fluorobenzonitrile (10.0 g, 50.0 mmol) in DMF (20 mL) was added. The reaction mixture was warmed to room temperature and stirred at 80° C. for 2 h, cooled to room temperature, and extracted with ethyl acetate (150 mL) and water (150 mL) The organic layer was washed with water (150 mL) and brine (150 mL), collected, dried over anhydrous sodium sulfate, filtered, and concentrated. The crude product was suspended with ethyl acetate:hexanes (1:3; 50 mL). The resulting suspension was stirred vigorously for 1 h, filtered, and dried. The mother liquor was concentrated and recrystallized. The crystals were combined and dried under vacuum to give the title compound (10.3 g). 1H NMR (DMSO-d6, 300 MHz) δ (ppm): 8.04 (dd, J=1.6, 8.2 Hz, 1H), 7.87 (dd, J=1.6, 7.6 Hz, 1H), 7.56-7.51 (m, 2H), 7.47-7.37 (m, 3H), 7.29 (t, J=7.9 Hz, 1H), 5.20 (s, 1H).

후처리

  1. temperatureThe reaction mixture was warmed to room temperature
  2. stirringstirred at 80° C. for 2 h
  3. temperaturecooled to room temperature
  4. extractionextracted with ethyl acetate (150 mL) and water (150 mL) The organic layer
  5. washwas washed with water (150 mL) and brine (150 mL)
  6. customcollected
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. stirringThe resulting suspension was stirred vigorously for 1 h
  11. filtrationfiltered
  12. customdried
  13. concentrationThe mother liquor was concentrated
  14. customrecrystallized
  15. customdried under vacuum

출처 및 근거

ORD 기록
ord-d76e311c097947988904ddda762caf02
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09199993B2

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