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tert-Butyl (R)-2-hydroxy-3-methylbutyrate synthesis
- Product Name:tert-Butyl (R)-2-hydroxy-3-methylbutyrate
- CAS Number:4216-96-0
- Molecular formula:C9H18O3
- Molecular Weight:174.24
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Yield:4216-96-0 200 g
Reaction Conditions:
Stage #1: tert-butyl alcoholwith copper chloride (I);diisopropyl-carbodiimide at 20; for 120 h;Inert atmosphere;
Stage #2: (R)-2-Hydroxy-3-methylbutyric acid in dichloromethane at 0 - 20; for 5 h;
Steps:
8-2 8-2) Synthesis of A-22-Int3
A solution of DIC (533 g, 4.23 mol) and CuCI (8 g, 0.08 mol) in t-BuOH (325.6 g, 4.4 mol) was stirred under nitrogen at room temperature for 5 days. The reaction was diluted with DCM (IL) . A-22-Int2 (200 g, 1.69 mol) was added to the solution in portion wise at 0°C. The reaction was stirred at room temperature for 5 hrs before filtering over a pad of celite. The filtrate was washed with saturated aqueous NazCCh and brine, then dried over with Na2SO4, concentrated and the residue was purified by distillation to afford A-22-Int3 (200 g) .XH NMR (400 MHz, CDCI3) data of A-22-Int3 is shown in Fig. 11
References:
WO2022/75486,2022,A1 Location in patent:Page/Page column 83; 84; 85
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