3-Methyl-1,3-butanediol synthesis
- Product Name:3-Methyl-1,3-butanediol
- CAS Number:2568-33-4
- Molecular formula:C5H12O2
- Molecular Weight:104.15
32368-09-5
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Yield:2568-33-4 97%
Reaction Conditions:
with [carbonylchlorohydrido{bis[2-(diphenylphosphinomethyl)ethyl]amino}ethylamino] ruthenium(II);potassium tert-butylate;hydrogen in tetrahydrofuran at 140; under 38002.6 Torr; for 12 h;Autoclave;
Steps:
19 Example 19: Hydrogenation of cyclic carbonate, 4,4-dimethyl-1,3-dioxan-2-one catalyzed by ruthenium complex1a
In a glove box, into a 125 mL autoclave was charged with ruthenium complex 1a (8.7 mg, 0.0143 mmol),potassium tert-butoxide (1.6 mg, 0.0143 mmol), tetrahydrofuran (20 mL) and 4,4-dimethyl-1,3-dioxan-2-one (3.32 g,28.6 mmol). The autoclave was sealed, removed from the glove box, and filled with hydrogen gas to 50 atm. The reactionvessel was heated in an oil bath at 140°C with stir for 12 hours. The reaction vessel was cooled in an ice-water bath for1.5 hours, and the excess of hydrogen was slowly deflated. The yield of methanol was determined as 99% with p-xyleneas internal standard by using gas chromatography. The separation yield of the diol is 97%.
References:
EP2910540,2015,A1 Location in patent:Paragraph 0095
