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ChemicalBook CAS DataBase List 2,2,6-Trimethyl-4H-1,3-dioxin-4-one

2,2,6-Trimethyl-4H-1,3-dioxin-4-one synthesis

14synthesis methods
-

Yield:5394-63-8 98%

Reaction Conditions:

with sulfuric acid;acetic anhydride at 0 - 20; for 5 h;

Steps:

1.1 Step - I: Preparation of 22.6-trimethyl-4H- I .-dioxin-4-one

To a solution of tert-butyl-3-oxobutnnnate (8.0 g. 50.6 mmoi) in acetone (50.0ml I cud aectic anhs di inc (0 0 i tki o ided d opcs lt on smpi nun It, id I: mU a50°C. Adler being stirred at ambient temperature for S h, the reaction mixiure was poured into I M 1-ICI and the aqueous laser was extracted with ethyl acetate. The combined organic layers were washed with saturated aqueous NaHCQ and brine, dried overintl tiltcied ltci temos ii nt it e sols u I the tes due s u ptiritiui hi columnchw n°itegi whs on ehe i l (0 to 30 % etns acetate in hexnne Ito attoid 2 2 6 n imeths I41’j-1,3-dioxin-4-one (7.0 g, 98%j as a colorless oil. 114 NMR (400 MHz, CDC13) 4 5.26(s 1H) 200 N 3Hi 1 70 (s 6H I3CMIR (100 MHz (DCI) o 1687 161 1 10u293.7, 24.9, 19.8; FT-lR (neat) cm’1 3000, 1739, 1640, 1393, 1358, 1273. 1206. 1032, 902.806 cm-I; MS: 143.3 M±IJ]’.

References:

WO2018/198086,2018,A1 Location in patent:Page/Page column 12

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