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Cyclopentanone → 4-(1-Hydroxycyclopentyl)benzoic acid

HRID 73004
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HRID 73004 반응식
Br[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.C([Li])CCC.[C:16]1(=[O:21])[CH2:20][CH2:19][CH2:18][CH2:17]1>O1CCCC1>[OH:21][C:16]1([C:2]2[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=2)[CH2:20][CH2:19][CH2:18][CH2:17]1
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참가 물질

5

반응물 3

HCID 8452CyclopentanoneHCID 114644-Bromobenzoic acidHCID 178418339Butyllithium

생성물 1

HCID 681537054-(1-Hydroxycyclopentyl)benzoic acid수율 30.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

A solution of 4-bromobenzoic acid (4.02 g, 20.0 mmol) in tetrahydrofuran (100 mL) was purged with argon for 5 min. n-Butyllithium (16.0 mL of 2.5 M in hexanes, 40 mmol) was added dropwise at −78° C., resulting in a yellow thick syrup. The mixture was stirred at −78° C. for 30 min. Cyclopentanone (3.89 mL, 44.0 mmol) was added dropwise. The reaction was quenched immediately with saturated NH4Cl and allowed to warm to room temperature. The mixture was acidified with 1 N HCl to pH ˜3 and extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine, dried over MgSO4 and concentrated in vacuo. The solid residue was suspended in hexanes, filtered, and the solid washed with additional hexanes. The solid was re-suspended in dichloromethane followed by hexanes. The resulting precipitate was filtered, washed with hexane and air dried to yield 4-(1-hydroxycyclopentyl)benzoic acid (1.25 g, 30%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 12.78 (s, 1H), 7.88 (d, J=8.5 Hz, 2H), 7.58 (d, J=8.5 Hz, 2H), 4.93 (s, 1H), 1.93-1.71 (m, 8H).

후처리

  1. additionwas added dropwise at −78° C.
  2. customresulting in a yellow thick syrup
  3. customThe reaction was quenched immediately with saturated NH4Cl
  4. temperatureto warm to room temperature
  5. extractionextracted with ethyl acetate (3×50 mL)
  6. washThe combined organic layers were washed with brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo
  9. filtrationfiltered
  10. washthe solid washed with additional hexanes
  11. filtrationThe resulting precipitate was filtered
  12. washwashed with hexane and air
  13. customdried

출처 및 근거

ORD 기록
ord-26460fcf96134848a0933e45c1bef0a1
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08828996B2

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