Ethylene Glycol → HCID 12869104、化合物

HRID 73622

反応式

HRID 73622 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 12869104HCID 12869104、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-e941809fc46f44f69bbcda672120d6df
出典データセット
uspto-grants-2014_09
特許番号
US08829196B2

関連ノート

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