反应详情

HATU (1.3 g, 3.5 mmol) was added to a solution of 3-amino-4-t-butoxycarbonylaminothiophene (Reference Compound No. 1-1, 0.68 g, 3.2 mmol), 5-methoxycarbonylpyridine-2-carboxylic acid (0.64 g, 3.5 mmol), and N-methylmorpholine (0.70 mL, 6.4 mmol) in DMF (20 mL), and then the reaction mixture was stirred at room temperature overnight. Water (0.30 L) and ethyl acetate (0.40 L) were added thereto, and the insoluble materials were filtered off to give 0.50 g of the title reference compound as a pale yellow solid. The filtrate was partitioned and the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and then the obtained solid was collected by filtration with ethylacetate (30 mL) to give 0.30 g of the title reference compound as a pale brown solid. (Yield 67%)

1. filtrationthe insoluble materials were filtered off
2. customto give 0.50 g of the title reference compound as a pale yellow solid
3. customThe filtrate was partitioned
4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. filtrationthe obtained solid was collected by filtration with ethylacetate (30 mL)
7. customto give 0.30 g of the title reference compound as a pale brown solid