1,4-Dioxaspiro[4.5]dec-7-ene, 7-methyl- synthesis
- Product Name:1,4-Dioxaspiro[4.5]dec-7-ene, 7-methyl-
- CAS Number:83313-55-7
- Molecular formula:C9H14O2
- Molecular Weight:154.21
Yield:83313-55-7 100%
Reaction Conditions:
with DL-10-camphorsulphonic acid at -10 - 0; for 0.5 h;Inert atmosphere;
Steps:
2 Preparation 2: 7-Methyl-1 ,4-dioxaspirof4.51dec-7-ene
A solution of Compound 2 (500 g, 4.03 mol) in DCM (4.0 L) was treated with (±)-10-camphorsulfonic acid (46.8 g, 201 mmol) and ethylene glycol (399 g, 6.04 mol) between about -10 °C and 0 °C. The mixture was stirred at about 0 °C for about 30 min. The reaction mixture was washed sequentially with sat. aq. NaHCOs (2 L) and then water (2 x 2 L), dried (Na2SC>4), filtered and concentrated to provide the title compound. Yield: 621 g (100%). 1H NMR (400 MHz, CDCh) 5 = 5.38 (td, 1 H), 3.95 (t, 4H), 2.21 - 2.12 (m, 6H), 1.67 (d, 3H).
References:
WO2022/130171,2022,A1 Location in patent:Page/Page column 47
