Acetic Anhydride → HCID 131725115, compound

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Reaction Steps

The product from Example 14 (120 mg, 0.150 mmol) was treated with N,N-diisopropylethylamine (0.13 mL, 5.0 eq) and acetic anhydride (30.6 mg, 2.0 eq) in dichloromethane (5 mL) at rt. After 1 h at rt, saturated NaHCO3 (5 mL) and ethyl acetate (100 mL) were added. The mixture was washed with water (2×5 mL), brine (5 mL), dried (MgSO4) and concentrated in vacuo. Purification by reverse phase HPLC (gradient elution, water/acetonitrile 80-20 to 20-80, 0.1% TFA) provided the title barbituric acid (75.4 mg, 69%). MS found: (M+H)+=502.

Provenance & Evidence