Ethylene Glycol → Ethyl (2-propyl-1,3-dioxolan-2-yl)acetate

HRID 31574

反応式

HRID 31574 の反応式
[O:1]=[C:2]([CH2:9][CH2:10][CH3:11])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH2:12](O)[CH2:13][OH:14].C(OCC)(OCC)OCC>O.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>[CH2:7]([O:6][C:4](=[O:5])[CH2:3][C:2]1([CH2:9][CH2:10][CH3:11])[O:14][CH2:13][CH2:12][O:1]1)[CH3:8]

参加物

6

反応物 3

HCID 174Ethylene GlycolHCID 31214Ethyl orthoformateHCID 238498Ethyl 3-oxohexanoate

生成物 1

HCID 14505110Ethyl (2-propyl-1,3-dioxolan-2-yl)acetate収率 97%

試薬・触媒・溶媒 2

HCID 521998p-Toluenesulfonic acid monohydrate触媒HCID 962Water溶媒

実験手順

A mixture of ethyl 3-oxohexanoate (5 g, 31.6 mmol), ethylene glycol (3.92 g, 63.2 mmol) and triethyl orthoformate (4.68 g, 31.6 mmol), and p-toluenesulfonic acid monohydrate (544 mg, 2.86 mmol) was stirred at room temperature for 29 hours and 10 minutes. To the reaction mixture, water was added and the mixture was extracted with ethyl acetate. The organic layer was washed with a saturated saline solution, dried over magnesium sulfate, and filtered. The filtrate was concentrated under reduced press-re to obtain the title compound (6.2 g, 97%) as a colorless oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with a saturated saline solution
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced press-re

出典と根拠

ORDレコード
ord-768326b17c3f4dd5bb13a20fb6733919
出典データセット
uspto-grants-2008_09
特許番号
US07425634B2

関連ノート

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