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

HRID 31574

반응식

HRID 31574 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 521998p-Toluenesulfonic acid monohydrate촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-768326b17c3f4dd5bb13a20fb6733919
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425634B2

연결된 노트

불러오는 중…