反应详情

(4-Morpholinyl)acetic acid trifluoroacetic acid salt (1.0 g) and thiosemicarbazide (0.25g) are heated in polyphosphoric acid (2.0 g) at 70° C. for 1 h. The mixture is cooled to room temperature and basified with sodium carbonate, which is extracted with CH2Cl2. The organic layer is dried (MgSO4), concentrated, and the residue is chromatographed (CH2Cl2/methanol, 9/1) to give 150 mg of the title compound as a white solid. Physical characteristics: MS (ESI+) m/z 201 (M+H)+.

1. extractionis extracted with CH2Cl2
2. dry with materialThe organic layer is dried (MgSO4)
3. concentrationconcentrated
4. customthe residue is chromatographed (CH2Cl2/methanol, 9/1)