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ChemicalBook CAS DataBase List tert-Butyl (R)-2-hydroxy-3-methylbutyrate

tert-Butyl (R)-2-hydroxy-3-methylbutyrate synthesis

7synthesis methods
-

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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