反应详情

To a suspension of 4-(3-isocyanato-benzyl)-2H-phthalazin-1-one (2)(1.4 g, 4.7 mmol) in dry DCM (40 ml) was added D-aspartic acid (0.455 g, 5.0 mmol), followed by triethylamine (1.4 ml, 10.0 mmol). The reaction was stirred at room temperature for 4 days. The reaction mixture was then filtered. The filtrate was then diluted with water (20 ml) and washed twice with DCM (2×20 ml). The combined DCM layers were dried over sodium sulfate and then concentrated in vacuo to afford a crude oil which was subjected to flash chromatography eluent neat ethyl acetate to remove impurity and the then 1:1 ethyl acetate/methanol to remove the desired component. (Rf of 0.2 in 1:1 ethyl acetate methanol). Single peak in LC-MS analysis, (0.79 g) requiring no further purification; m/z (LC-MS, ESP), RT=2.70 (M+H) 384;

1. filtrationThe reaction mixture was then filtered
2. additionThe filtrate was then diluted with water (20 ml)
3. washwashed twice with DCM (2×20 ml)
4. dry with materialThe combined DCM layers were dried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customto afford a crude oil which
7. customto remove impurity
8. customthe then 1:1 ethyl acetate/methanol to remove the desired component
9. customno further purification
10. customm/z (LC-MS, ESP), RT=2.70 (M+H) 384