(R)-3-HYDROXYGLUTARATE ETHYL TERT-BUTYL synthesis
- Product Name:(R)-3-HYDROXYGLUTARATE ETHYL TERT-BUTYL
- CAS Number:128237-30-9
- Molecular formula:C11H20O5
- Molecular Weight:232.27
Yield:128237-30-9 76.5%
Reaction Conditions:
with thionyl chloride in dichloromethane at 0 - 20;
Steps:
1 Example 1. Preparation of compound of formula 4 (R2 is ethyl)
Stirring device,3,000 mL with a thermometerIn a round flask, a monoester compound (compound of formula 3)And dichloromethaneWere added. The temperature of the reactants 0 AndSOCl2 266.09 gAfter that,The reactantsThe temperature was raised to 20 ° C, and 552.59 g of t-butanol was added to the reaction product. At this time, the progress of the reaction was confirmed by TLC (Thin Layer Chromatography;Eluent: n-hexane / ethyl acetate, 1/1). When the reaction was completed with stirring at this temperature, 1,000 g of distilled water was slowly added to the reaction product. The reaction mixture was stirred for 15 minutes and then the water layer and the organic layer were separated. The solvent and the low boiling point organic compound were recovered by distillation from the organic layer and distilled under reduced pressure to obtain a diester compound (yield: 76.5%, purity: 98.0% Chiral purity: 99.8%).
References:
KR2016/120532,2016,A Location in patent:Paragraph 0177-0178
