Propylene carbonate synthesis
- Product Name:Propylene carbonate
- CAS Number:108-32-7
- Molecular formula:C4H6O3
- Molecular Weight:102.09
57-55-6
1555 suppliers
$5.00/1g
124-38-9
129 suppliers
$214.00/14L
115-19-5
261 suppliers
$17.00/25mL
108-32-7
604 suppliers
$7.00/100g
115-22-0
124 suppliers
$9.00/1g
Yield:108-32-7 95% ，115-22-0 67 %Chromat.
Reaction Conditions:
with 1,8-diazabicyclo[5.4.0]undec-7-ene;zinc(II) chloride in acetonitrile at 80; under 7500.75 Torr; for 24 h;Mechanism;Autoclave;Sealed tube;chemoselective reaction;
Steps:
4-Methyl-1,3-dioxolan-2-one (5a); Typical Procedure (Table 2)
General procedure: A 50-mL stainless steel autoclave equipped with a magnetic stir bar was charged with ZnCl2 (27.2 mg, 20 mol%), DBU (76 mg, 50 mol%), 4a (76.1 mg, 1 mmol), 2a (126.1 mg, 1.5 mmol), and CH3CN (2.0 mL) successively and sealed at r.t. The pressure was adjusted to 1 MPa with CO2 at the preset temperature (80 °C) and the autoclave was heated at this temperature for 24 h. After the reaction was complete, the reactor was cooled in ice-water bath, and then excess CO2 was carefully vented. The mixture was diluted with EtOAc, and the yield of cyclic carbonate 5a and α-hydroxy ketone 6a was determined by gas chromatograph (Agilent 6890) equipped with a capillary column (HP-5 30 m * 0.25 μm) using a flame ionization detector using biphenyl (40 mg) as the internal standard. Then, the residue was obtained by removing the solvent under vacuum and further purified by column chromatography (petroleum ether/EtOAc 100:1-5:1) to obtain 5a and 6a. 4-Methyl-1,3-dioxolan-2-one (5a) Colorless liquid; yield: 98 mg (95%). 1H NMR (400 MHz, CDCl3): δ = 4.84-4.92 (m, 1 H), 4.58 (t, J = 8.4 Hz, 1 H), 4.04 (t, J = 8.4 Hz, 1 H), 1.49 (d, J = 6.0 Hz, 3 H). 13C{1H} NMR (100.6 MHz, CDCl3): δ = 155.1, 73.7, 70.7, 19.4.
References:
Song, Qing-Wen;Zhao, Qing-Ning;Li, Jing-Yuan;Zhang, Kan;Liu, Ping [Synthesis,2019,vol. 51,# 3,p. 739 - 746]
57-55-6
1555 suppliers
$5.00/1g
124-38-9
129 suppliers
$214.00/14L
108-32-7
604 suppliers
$7.00/100g
127-66-2
159 suppliers
$11.00/1g
57-55-6
1555 suppliers
$5.00/1g
124-38-9
129 suppliers
$214.00/14L
108-32-7
604 suppliers
$7.00/100g
3155-01-9
1 suppliers
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