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L-Valine (200 g, 1.7 mol eq) is dissolved in water (500 mL) followed by the addition of NaOH (30%, 170 mL). The mixture is cooled to 0-5C followed by the addition of acetic anhydride (32 ml, 1.4 eq. ). Sodium hydroxide (30%, 34 mL) is added while keeping the temperature at 0-5C. Acetic anhydride and 30% NaOH alternate additions are repeated six time while keeping the temperature (acetic anhydride, 6 x 32 mL; 30% NaOH 6 x 34 mL). After all the additions are completed, the mixture is stirred for an additional two hours at 0C. Hydrochloric acid (32%, 380 mL) is added to lower the pH below 3 while keeping the temperature at 0C. The resulting slurry is granulated for 12 hours, filter and the cake washed with HCI (0.1 N, 100 mL). The wet N-acetyl-L-valine was dried to produce 233 g (86% yield).
Step 1. After compound 41-1 (470.6 mg, 4 mmol) in water (10 mL) was sonicated for 6 min, Ac20 was added over 4 min. The mixture was concentrated and the residue was dissolved in MeOH, filtered, concentrated to give crude 41-2 as a white solid (350 mg, 55%). 'H NMR DMSO-^ 400 MHz, delta 7 '.94 - 7.92 (d, J= 8.0 1 H), 4.10 - 4.08 (m, 1H), 2.01 - 1.99 (m, 1 H), 1.84 (s, 1 H), 0.83 - 0.80 (m, 6 H)
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