反应详情

The product of Example 308A (604 mg, 2.35 mmol) and HOOBT (574 mg, 3.52 mmol) were dissolved in DMF (10 mL) and methionine methyl ester HCl (679 mg, 3.52 mmol) and EDCI (676 mg, 3.52 mmol) were added followed by Et3N (476 mg, 0.65 mL, 4.7 mmol). The reaction was stirred for 12 hours and then was taken up in ethyl acetate and washed successively with brine (3×) and water (3×). The ethyl acetate layer was dried over Na2SO4, filtered and evaporated. Purification by chromatography on silica gel (5% methanol-ethyl acetate) gave the desired compound (940 mg, 98%).

1. washwashed successively with brine (3×) and water (3×)
2. dry with materialThe ethyl acetate layer was dried over Na2SO4
3. filtrationfiltered
4. customevaporated
5. customPurification by chromatography on silica gel (5% methanol-ethyl acetate)