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Bromoacetic Acid → 2-(1-(4-Bromophenyl)cyclopentyloxy)acetic acid

HRID 1397491
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HRID 1397491 반응식
[H-].[Na+].[Br:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2([OH:15])[CH2:14][CH2:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.Br[CH2:17][C:18]([OH:20])=[O:19]>CN(C)C=O>[Br:3][C:4]1[CH:5]=[CH:6][C:7]([C:10]2([O:15][CH2:17][C:18]([OH:20])=[O:19])[CH2:14][CH2:13][CH2:12][CH2:11]2)=[CH:8][CH:9]=1
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참가 물질

5

반응물 3

HCID 6227Bromoacetic AcidHCID 24758Sodium hydrideHCID 231542891-(4-Bromophenyl)cyclopentan-1-ol

생성물 1

HCID 687203352-(1-(4-Bromophenyl)cyclopentyloxy)acetic acid

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

To an ambient suspension of NaH (332 mg, 8.30 mmol, 60 wgt % in mineral oil) in N,N-dimethylformamide (2 mL) was added dropwise a solution of Example 30A (1.0 g, 4.15 mmol) in N,N-dimethylformamide (1 mL). After 30 min., bromoacetic acid (577 mg, 4.15 mmol) in N,N-dimethylformamide (13 mL) was added, dropwise. The solution was stirred at room temperature for 16 h and then heated to 50° C. for 3 h. The reaction was cooled to room temperature and was quenched by the addition of water (10 mL). The solution was basicified to pH 10 by the addition of 2.5 M NaOH. The aqueous was extracted with ethyl acetate (2×10 mL), and the organics discarded. The aqueous was acidified to pH 1 with 6 M HCl, and then extracted with ethyl acetate (3×10 mL). The combined organics were washed with water (3×10 mL), brine (1×10 mL), dried over sodium sulfate, filtered, and concentrated, under reduced pressure to give the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.66-1.72 (m, 2 H), 1.74-1.85 (m, 4 H), 2.02-2.15 (m, 2 H), 3.56-3.60 (m, 2 H), 7.33-7.39 (m, 2 H), 7.49-7.56 (m, 2 H), 12.37 (s, 1 H).

후처리

  1. temperatureheated to 50° C. for 3 h
  2. temperatureThe reaction was cooled to room temperature
  3. customwas quenched by the addition of water (10 mL)
  4. additionThe solution was basicified to pH 10 by the addition of 2.5 M NaOH
  5. extractionThe aqueous was extracted with ethyl acetate (2×10 mL)
  6. extractionextracted with ethyl acetate (3×10 mL)
  7. washThe combined organics were washed with water (3×10 mL), brine (1×10 mL)
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated, under reduced pressure

출처 및 근거

ORD 기록
ord-e332745ffef84ba7ab0b961972adabaf
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901152B2

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