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 2-Propenoic acid, 2-methyl-, 6-hydroxyhexyl ester

2-Propenoic acid, 2-methyl-, 6-hydroxyhexyl ester synthesis

6synthesis methods
-

Yield:13092-57-4 67.7% ,6606-59-3 15%

Reaction Conditions:

with 2,6-di-tert-butyl-4-methyl-phenol;toluene-4-sulfonic acid at 90; for 5 h;

Steps:



6-Hydroxyhexyl Methacrylate Synthesis: 1,6-Hexanediol (1000.00 g, 8.46 mol, Sigma-Aldrich) was placed in a 1 -liter 3 -neck flask equipped with a mechanical stirrer and a narrow tube blowing dry air into the flask. The solid diol was heated to 900C, at which temperature all the solid melted. With continuous stirring, p-toluenesulfonic acid crystals (18.95 g, 0.11 mol) followed by BHT (2.42 g, 0.011 mol) and methacrylic acid (728.49.02 g, 8.46 mol). Heating at 9O0C with stirring was continued for 5 hours during which time vacuum was applied using tap water aspirator for 5-10 minutes after each half- hour reaction time. The heat was turned off and the reaction mixture was cooled to room temperature. The viscous liquid obtained was washed with 10% aqueous sodium carbonate twice (2 x 240 ml), followed by washing with water (2 x 240 ml), and finally with 100 ml of saturated NaCl aqueous solution. The obtained oil was dried using anhydrous Na2SO4 EPO then isolated by vacuum filtration to give 1067 g (67.70 %) of 6-hydroxyhexyl methacrylate, a yellow oil. This desired product was formed along with 15-18% of 1,6- bis(methacryloyloxyhexane). Chemical characterization was by NMR analysis.

References:

WO2006/55317,2006,A1 Location in patent:Page/Page column 30-31