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Ethylene Glycol → Methyl 8-methyl-1,4-dioxaspiro[4.5]decane-8-carboxylate

HRID 1462922
ノート
印刷プレビュー

反応式

HRID 1462922 の反応式
[CH3:1][C:2]1([C:9]([O:11][CH3:12])=[O:10])[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][CH2:3]1.[CH2:13](O)[CH2:14][OH:15].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1C=CC=CC=1>[CH2:13]1[CH2:14][O:15][C:5]2([CH2:4][CH2:3][C:2]([CH3:1])([C:9]([O:11][CH3:12])=[O:10])[CH2:7][CH2:6]2)[O:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 962WaterHCID 521998p-Toluenesulfonic acid monohydrateHCID 12568255Methyl 1-methyl-4-oxocyclohexane-1-carboxylate

生成物 1

HCID 22591390Methyl 8-methyl-1,4-dioxaspiro[4.5]decane-8-carboxylate収率 100%

試薬・触媒・溶媒 1

HCID 241Benzene
このページの内容参加物実験手順後処理出典と根拠反応ノート
溶媒

実験手順

Methyl 1-methyl-4-oxocyclohexanecarboxylate (30 g) was dissolved in benzene (300 ml). Ethylene glycol (30 ml) and p-toluenesulfonic acid monohydrate (1 g) were added, and the mixture was refluxed for 4 hours. The water which formed during the heating was removed by using a water trap. After cooling, the mixture was washed with water and dryed (MgSO4). The solvent was distilled off to give methyl 4,4-ethylenedioxy-1-methylcyclohexanecarboxylate as an oil (37.8 g, 100%).

後処理

  1. temperaturethe mixture was refluxed for 4 hours
  2. customwas removed
  3. temperatureAfter cooling
  4. washthe mixture was washed with water
  5. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-2f9cab8403a347f594ea664526428688
出典データセット
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04461902

反応ノート

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