反应详情

温度

150 °C

To a vial containing the title compound from Example 71 Step D (75 mg, 0.217 mmol), acetamide oxime (32.1 mg, 0.433 mmol) and sodium ethoxide (73.7 mg, 1.083 mmol) was added ethanol (2.2 mL). The vial was capped tightly and heated to 150° C. for 15 minutes in the microwave. The reaction solution was then concentrated under reduced pressure. The resulting material was diluted with acetonitrile and then purified by HPLC (C18 column, 10 to 100% acetonitrile/water, both 0.1% v/v trifluoroacetic acid). Fractions containing product were combined, aqueous 1 N HCl solution was added, and the resulting solution concentrated to provide the title compound: LCMS m/z 370.97 [M+H]+; 1H NMR (500 MHz, CD3OD) δ 10.1 (s, 1H), 9.28 (s, 1H), 9.13 (s, 1H), 8.1-8.01 (m, 4H), 3.49-3.46 (m, 2H), 3.39-3.36 (m, 2H), 2.29 (s, 3H), 2.04-2.02 (m, 2H), 1.94-1.91 (m, 2H).

1. customThe vial was capped tightly
2. concentrationThe reaction solution was then concentrated under reduced pressure
3. additionThe resulting material was diluted with acetonitrile
4. custompurified by HPLC (C18 column, 10 to 100% acetonitrile/water
5. additionFractions containing product
6. additionaqueous 1 N HCl solution was added
7. concentrationthe resulting solution concentrated