diethyl 2-oxaspiro[3.3]heptane-6,6-dicarboxylate synthesis
- Product Name:diethyl 2-oxaspiro[3.3]heptane-6,6-dicarboxylate
- CAS Number:26593-41-9
- Molecular formula:C12H18O5
- Molecular Weight:242.27
Yield:26593-41-9 15.4%
Reaction Conditions:
Stage #1: 3,3-bis(chloromethyl)oxetane;methanetricarboxylic acid triethyl ester in ethanol;Reflux;
Stage #2: with sodium ethanolate in ethanol; for 18 h;Reflux;
Steps:
10.3 Step 3: Diethyl 2-oxaspiro [3,3] heptane-6,6-dicarboxylate
3,3-bis (chloromethyl) oxetane obtained from the above step 2(7.59 g, 48.96 mmol) and tris (ethoxycarbonyl) methane (47.5 g, 205 mmol) were added to ethanol (100 ml) and heated to reflux.A 21% sodium ethoxide / ethanol solution (15 ml) was slowly added to the reaction solution. The reaction solution was heated to reflux for 18 hours and then cooled to room temperature. The resulting solid was filtered off and the filtrate was concentrated under reduced pressure to remove the solvent. Water was added to the residue, and the mixture was extracted twice with diethyl ether. The obtained organic layers were combined, washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure.The resulting residue was purified by silica gel column chromatography (hexane: ethyl acetate = 9: 1 and 2: 1) to give pure diethyl 2-Oxaspiro [3,3] heptane-6,6-dicarboxylate (1.83 g, 15.4%).
References:
KR101592370,2016,B1 Location in patent:Paragraph 0204; 0205; 0213-0215
13103-49-6
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