Ethylene Glycol → HCID 12869104, 화합물

HRID 73622

반응식

HRID 73622 반응식
[CH3:1][O:2][C:3]([CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C:6]1=[O:11])=[O:4].[CH2:12](O)[CH2:13][OH:14].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1>[O:14]1[C:6]2([CH2:7][CH2:8][CH2:9][CH2:10][CH:5]2[C:3]([O:2][CH3:1])=[O:4])[O:11][CH2:12][CH2:13]1

참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 170489Cyclohexanecarboxylic acid, 2-oxo-, methyl esterHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 12869104HCID 12869104, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of methyl-2-oxocyclohexanecarboxylate (4-1) (7.0 g, 44.8 mmol), ethylene glycol (3.00 mL, 53.8 mmol) and p-toluenesulfonic acid monohydrate (0.853 g, 4.48 mmol) in Benzene (45 mL) was heated to reflux overnight. The reaction was then cooled to rt and concentrated. The residue was purified by column chromatography to give the title compound. 1H NMR (500 MHz, CDCl3) δ 3.86-3.99 (m, 4H), 3.69 (s, 3H), 2.69 (dd, 1H, J=4.9 Hz, 9.0 Hz), 1.82-1.97 (m, 3H), 1.58-1.73 (m, 3H), 1.45-1.53 (m, 1H), 1.26-1.37 (m, 1H).

후처리

  1. temperaturewas heated
  2. temperatureto reflux overnight
  3. concentrationconcentrated
  4. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-e941809fc46f44f69bbcda672120d6df
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829196B2

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