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Potassium Hydroxide → HCID 11738543, 화합물

HRID 661148
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HRID 661148 반응식
C(C1C=C[C:8]([C:11]([CH3:40])([CH2:15][CH2:16][CH2:17][CH2:18][C:19](=[O:39])[CH2:20][CH2:21][CH2:22][CH2:23][C:24]([C:29]2C=CC(CC(C)C)=CC=2)([CH3:28])[C:25]([OH:27])=[O:26])[C:12]([OH:14])=[O:13])=CC=1)C(C)C.[OH-].[K+]>C(O)C.O>[O:39]=[C:19]([CH2:20][CH2:21][CH2:22][CH2:23][C:24]([CH3:29])([CH3:28])[C:25]([OH:27])=[O:26])[CH2:18][CH2:17][CH2:16][CH2:15][C:11]([CH3:8])([CH3:40])[C:12]([OH:14])=[O:13]
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참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 103252762,12-Bis-(4-isobutylphenyl)-2,12-dimethyl-7-oxotridecanedioic acid

생성물 1

HCID 11738543HCID 11738543, 화합물수율 86%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

According to the procedure given for 210f, 209c (30.0 g, 81.0 mmol) was saponified with KOH (85%, 18.9 g, 286 mmol) in ethanol (143 mL) and water (48 mL) at reflux for 5 h. The solid product obtained after extraction and drying was purified by flash chromatography (silica; hexanes/ethyl acetate=90/10) to afford 210c (22.0 g, 86%) as a white solid. Mp 60-61.5° C. 1H NMR (CDCl3): δ 11.40 (br., 2H), 2.41 (t, 4H, J=7.3), 1.62-1.48 (m, 8H), 1.32-1.18 (m, 4H), 1.18 (s, 12H). 13C NMR (CDCl3=77.0 ppm): δ 211.11, 184.74, 42.49, 42.14, 40.42, 24.92, 24.62, 23.99. HRMS (LSIMS, gly): Calcd for C17H31O5 (MH+): 315.2171. found: 315.2183. HPLC: 94.5% pure. Anal. (C17H30O5) C, H.

후처리

  1. temperatureat reflux for 5 h
  2. customThe solid product obtained
  3. extractionafter extraction
  4. customdrying
  5. customwas purified by flash chromatography (silica; hexanes/ethyl acetate=90/10)

출처 및 근거

ORD 기록
ord-9b847b245c4a473a97e17ba1bad4a407
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084498B2

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