5-Isobenzofurancarboxylic acid, 1,3-dihydro-1,3-dioxo-, 5,5'-[(1-methylethylidene)di-4,1-phenylene] ester synthesis
- Product Name:5-Isobenzofurancarboxylic acid, 1,3-dihydro-1,3-dioxo-, 5,5'-[(1-methylethylidene)di-4,1-phenylene] ester
- CAS Number:2770-50-5
- Molecular formula:C33H20O10
- Molecular Weight:576.51
Yield:-
Reaction Conditions:
lithium acetate in diphenylether at 210; for 7 h;Product distribution / selectivity;Inert atmosphere;
Steps:
1
(Example 1) A 300-ml four-way flask equipped with an agitator, thermometer, Dean-Stark and reflux condenser was replaced with nitrogen, after which 25.0 g (0.080 mol) of BPA-DA obtained in Reference Example 1, 46.2 g (0.241 mol) of trimellitic anhydride, 0.25 g (4.7 mol percent relative to BPA-DA) of lithium acetate and 54.5 g of diphenyl ether were introduced to the flask. Next, the mixture was heated to 210°C under nitrogen flows to cause reaction at 210°C under agitation. The mixture was heated to 210°C under nitrogen flows at normal pressure, and then kept at that temperature for 7 hours to cause reaction. During the reaction, produced acetic acid was removed by distillation as the reaction progressed. Reaction solution was sampled 4 hours and 7 hours after the mixture had been heated to 210°C, and analyzed by GPC (gel permeation chromatography). The results are shown in Table 1. The reaction selectivity of 2,2-bis {4-(1,3-dioxo-1,3-dihydroisobenzofuran-5-ylcarbonyloxy)phenyl}propane, which is the target substance (bistrimellitic anhydride), was 96.7%.
References:
Honshu Chemical Industry Co., Ltd. EP2383265, 2011, A1 Location in patent:Page/Page column 8
80-05-7
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