反应详情

温度

95 °C

To a solution of the product of Step A, cyanoacetamide (1.33 g, 15.8 mmol), and MeOH (1.3 mL, 32 mmol) in DMF (35 mL) was added dropwise to a suspension of NaH (60% in mineral oil) (1.45 g, 36 mmol) in DMF (16 mL) at rt. After the slow addition was complete, the reaction was heated to 95° C. for 2.5 h. Most of the DMF was then removed in vacuo before the reaction was diluted with aq 18% citric acid solution. The mixture was extracted twice with CH2Cl2 and the organic layers were washed with brine. The combined organic layers were dried (Na2SO4) and concentrated. The solid residue was triturated with ether, filtered, and air dried to afford the product. (LC-2) HPLC/MS: 375 (M+1), 377 (M+3); Rt=3.47 min.

1. additionAfter the slow addition
2. customMost of the DMF was then removed in vacuo before the reaction
3. additionwas diluted with aq 18% citric acid solution
4. extractionThe mixture was extracted twice with CH2Cl2
5. washthe organic layers were washed with brine
6. dry with materialThe combined organic layers were dried (Na2SO4)
7. concentrationconcentrated
8. customThe solid residue was triturated with ether
9. filtrationfiltered
10. customair dried
11. customto afford the product