(2,2,5-TRIMETHYL-[1,3]DIOXAN-5-YL)METHANOL synthesis
- Product Name:(2,2,5-TRIMETHYL-[1,3]DIOXAN-5-YL)METHANOL
- CAS Number:3663-46-5
- Molecular formula:C8H16O3
- Molecular Weight:160.21
77-85-0
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Yield: 98%
Reaction Conditions:
with toluene-4-sulfonic acid at 20; for 48 h;Inert atmosphere;
Steps:
1.1.8 17FM025:
In a round bottom flask were introduced tris(hydroxymethyl)ethane (2 g, 16.7 mmol) and a catalytic quantity of PTSA (2 mg) in acetone under inert atmosphere. The mixture was stirred at room temperature for 2 days. The reaction was neutralized with 50mg of K2C03, filtrated and evaporated to give the desired product with 96% of purity. mpure = 2.64 g. Aspect: colorless oil. Yield: 98%. 1H NMR (500 MHz, DMSO) d (ppm): 4.57 (t, 1 H, J = 5.4 Hz), 3.49 (AB system, 2H, J = 1 1.7 Hz), 3.44 (AB system, 2H, J = 1 1 .7 Hz), 3.35 (d, 1 H, J = 5.3 Hz), 1 .33 (s, 3H), 1 .27 (s, 3H), 0.75 (s, 3H). 13C {1H} NMR (126 MHz, DMSO) d (ppm): 96.92, 65.34 (2x), 63.61 , 34.22, 25.80, 21.57, 17.61
References:
UNIVERSITé DE BOURGOGNE;INSERM (INSTITUT NATIONAL DE LA SANTé ET DE LA RECHERCHE MéDICALE);KHAN, Naim;JUGE, Sylvain;HICHAMI, Aziz;BAYARDON, Jér?me;MANGIN, Floriane;KHAN, Amira WO2019/228994, 2019, A1 Location in patent:Page/Page column 33-34
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