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Methanol → 3-Cyano-3-(4-hydroxyphenyl)propanoic acid

HRID 922190
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HRID 922190 반응식
CO.C(OC(=O)[C:7](=[CH:13][C:14]1[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=1)[C:8]([O:10]CC)=[O:9])C.[C-:22]#[N:23].[K+]>O>[C:22]([CH:13]([C:14]1[CH:15]=[CH:16][C:17]([OH:20])=[CH:18][CH:19]=1)[CH2:7][C:8]([OH:10])=[O:9])#[N:23]
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참가 물질

5

반응물 3

HCID 887MethanolHCID 9032Potassium CyanideHCID 576572Diethyl 2-(4-hydroxybenzylidene)malonate

생성물 1

HCID 666854583-Cyano-3-(4-hydroxyphenyl)propanoic acid수율 72.3%

시약·촉매·용매 1

HCID 962Water용매

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온도
70 °C

실험 절차

To a 25 mL RB flask fitted with magnetic stirrer was charged with methanol (6 mL) and water (1 mL). To the stirred solvent was added 2-(4-hydroxy-benzylidene)-malonic acid diethyl ester (1 g, 3.8 mmol), followed by potassium cyanide (0.492 g, 7.6 mmol). The RM was heated at 70° C. for 2 h. The RM was concentrated, diluted with saturated NaHCO3 solution (50 mL) and washed with ethyl acetate (50 mL×2). The aqueous layer was acidified to pH 3 with 1N hydrochloric acid and extracted with ethyl acetate (50 mL×2). The organic layer was washed with water (50 mL) and saturated brine solution (50 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The product was obtained as brown liquid. (0.6 g, yield: 72.3%); MS (ESI, 120 eV): m/z=190.0 (M−H)+; 1H NMR (300 MHz, DMSO-d6): δ 12.69 (s, 1H), 9.58 (s, 1H), 7.22-7.24 (d, 2H), 6.75-6.78 (d, 2H), 4.28-4.40 (m, 1H), 2.77-3.12 (m, 2H).

후처리

  1. customTo a 25 mL RB flask fitted with magnetic stirrer
  2. concentrationThe RM was concentrated
  3. additiondiluted with saturated NaHCO3 solution (50 mL)
  4. washwashed with ethyl acetate (50 mL×2)
  5. extractionextracted with ethyl acetate (50 mL×2)
  6. washThe organic layer was washed with water (50 mL) and saturated brine solution (50 mL)
  7. dry with materialThe organic layer was dried over anhydrous Na2SO4
  8. customthe solvent was removed under reduced pressure
  9. customThe product was obtained as brown liquid

출처 및 근거

ORD 기록
ord-59a9a04257e342729c542655394221d6
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278915B2

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