Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 1,9-Dihydroxy-3,7-dioxanonane, 2,2μ-(Trimethylenedioxy)diethanol

1,9-Dihydroxy-3,7-dioxanonane, 2,2μ-(Trimethylenedioxy)diethanol synthesis

10synthesis methods
77319-28-9 Synthesis
Acetic acid, 2,2'-[1,3-propanediylbis(oxy)]bis-, diethyl ester (9CI)

77319-28-9
0 suppliers
inquiry

-

Yield: 90%

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran at 0 - 10; for 1 h;

Steps:

2 Step 2-2-[3-(2-Hydroxyethoxy)propoxy]ethanol
To a solution of ethyl 2-[3-(2-ethoxy-2-oxo-ethoxy)propoxy]acetate (20.0 g, 80.5 mmol) in THF (300 mL) was added LiAlH4 (6.24 g, 161 mmol, 98% purity) at 0° C. The mixture was then stirred at 10° C. for 1 hour. On completion, the mixture was quenched with water (10 mL) and NaOH aqueous solution (15%, 10 mL) at 0° C., and the reaction was filtered. The filtrate was dried over Na2SO4, filtered and concentrated in vacuo to give the title compound (12 g, 90% yield) as colourless oil. 1H NMR (400 MHz, DMSO-d6) δ 4.53 (t, J=5.2 Hz, 2H), 3.50-3.45 (m, 4H), 3.43 (t, J=6.4 Hz, 4H), 3.37 (t, J=5.2 Hz 4H), 1.75-1.68 (m, 2H)

References:

Kymera Therapeutics, Inc.;Mainolfi, Nello;Ji, Nan;Kluge, Arthur F.;Weiss, Matthew M.;Zhang, Yi US2019/192668, 2019, A1 Location in patent:Paragraph 3132; 3134

1,9-Dihydroxy-3,7-dioxanonane, 2,2μ-(Trimethylenedioxy)diethanol Related Search: