2-methylenepropane-1,3-diyl diacetate synthesis
- Product Name:2-methylenepropane-1,3-diyl diacetate
- CAS Number:3775-29-9
- Molecular formula:C8H12O4
- Molecular Weight:172.18
Yield: 7.3 g
Reaction Conditions:
with oxygen at 140; under 15201 Torr; for 5 h;Autoclave;Concentration;
Steps:
31; 9; 10; 81 Example 31
1.3 g of catalyst 2, 40 g (666 mmol) of acetic acid and 8 g (70 mmol) of methallyl acetate were charged to an electromagnetic stirring autoclave having an internal volume of 100 mL provided with a gas inlet and a sampling port, and the inside of the autoclave was brought to 20 atm (gauge pressure) with a mixed gas of oxygen/nitrogen=8/92 (molar ratio), and then the temperature in the autoclave was raised to 140° C. with stirring. Then, the reaction was carried out for 5 hours while flowing a mixed gas at a flow rate of 200 mL/min and maintaining 90 atm (gauge pressure) with a mixed gas of oxygen/nitrogen=8/92 (molar ratio). The conversion of methallyl acetate was 99%, and the selectivity to 1,3-diacetoxy-2-methylenepropane was 61%. The yield of 1,3-diacetoxy-2-methylenepropane was 7.3 g (42 mmol), and the production efficiency of 1,3-diacetoxy-2-methylenepropane was 1.14 g (product)/{g(catalyst)·hr}.
References:
KURARAY CO., LTD.;MURATA, Yusuke;MINAMOTO, Naoya;KANEKO, Mitsumasa;SHIMIZU, Ryosuke US2020/283367, 2020, A1 Location in patent:Paragraph 0101; 0109-0115
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