Allyl chloride → 2,5,8,11-Tetraoxatetradec-13-ene

540 mls of dried peroxide free tetrahydrofuran and 21.5 g of potassium metal are charged into a 2000 ml three-neck flask equipped with mechanical stirrer and a dry nitrogen inlet. 88.4 ml of triethylene glycol monomethyl ether, available from Chemical Samples Co., is added to the mixture dropwise. After the potassium metal has completely reacted, 48.6 ml of allyl chloride is added dropwise to the mixture at such a rate in order to maintain a gentle reflux. After the reaction is complete, 500 mls of distilled water are added in order to dissolve the precipitated salt. The tetrahydrofuran layer is washed with salt water (270 g NaCl/l liter water) in order to remove the excess alcohol. The resulting product in tetrahydrofuran is collected and the tetrahydrofuran is removed with a water aspirator. The product is distilled at reduced pressure. 75.5 g (74% yield) of triethylene glycol allyl methyl ether is obtained (b.p. 97° C.-100° C./ 2 mm.). The analytical data is consistent with a product of the general formula:

1. customequipped with mechanical stirrer and a dry nitrogen inlet
2. addition, is added to the mixture dropwise
3. temperatureto maintain a gentle reflux
4. dissolutionto dissolve the precipitated salt
5. washThe tetrahydrofuran layer is washed with salt water (270 g NaCl/l liter water) in order
6. customto remove the excess alcohol
7. customThe resulting product in tetrahydrofuran is collected
8. customthe tetrahydrofuran is removed with a water aspirator
9. distillationThe product is distilled at reduced pressure

ORD 기록

ord-c24b5c6578c945b19e4c1975671cb509

출처 데이터셋

uspto-grants-1981_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04260725