Ethylene Glycol → Ethyl 1,4-dioxaspiro(4.5)decane-8-carboxylate

HRID 12639

反応式

HRID 12639 の反応式
[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][CH2:10][C:9](=[O:12])[CH2:8][CH2:7]1)=[O:5])[CH3:2].[CH2:13](O)[CH2:14][OH:15].C1(C)C=CC(S(O)(=O)=O)=CC=1.C(OCC)C>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][CH2:10][C:9]2([O:15][CH2:14][CH2:13][O:12]2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 3283Diethyl EtherHCID 6101p-Toluenesulfonic acidHCID 317638Ethyl 4-oxocyclohexanecarboxylate

生成物 1

HCID 10488810Ethyl 1,4-dioxaspiro(4.5)decane-8-carboxylate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-oxo-cyclohexanecarboxylic acid ethyl ester (52.8 g, 0.31 mole, Merck, Order No. 814249), ethylene glycol (67.4 g, 1.08 mole) and p-toluenesulfonic acid (0.7 g) in toluene (160 ml) were stirred for 20 hours at RT, and the reaction solution was poured into diethyl ether (300 ml) and washed with water, sodium hydrogen carbonate solution and sodium chloride solution. The solution was dried (Na2SO4), concentrated by evaporation in vacuo, and the remaining colorless liquid was processed further without purification.

後処理

  1. washwashed with water, sodium hydrogen carbonate solution and sodium chloride solution
  2. dry with materialThe solution was dried (Na2SO4)
  3. concentrationconcentrated by evaporation in vacuo
  4. customthe remaining colorless liquid was processed further without purification

出典と根拠

ORDレコード
ord-cf51c88887784dd4a140c68d1eeaed7a
出典データセット
uspto-grants-2010_06
特許番号
US07728028B2

関連ノート

読み込み中…