反应详情

温度

100 °C

Preparation I6, Step 2: A solution of 5-(trifluoromethyl)-1H-indazol-3-amine (2.08 g, 10.3 mmol) in 50 mL of 1% AcOH/MeOH was charged with ethyl glyoxylate (2.05 mL of a 50% solution in toluene, 10.3 mmol; note: the commercially available material is polymeric and was heated at 100° C. for 90 min before being used immediately in this reaction) and sodium cyanoborohydride (777 mg, 12.4 mmol). The mixture was stirred for 2.5 h, quenched with sat. NaHCO3, and extracted with EtOAc (2×). The organic extracts were combined, washed with brine, dried (sodium sulfate), filtered, and concentrated in vacuo. Purification by flash chromatography provided ethyl 2-(5-(trifluoromethyl)-1H-indazol-3-ylamino)acetate (819 mg).

1. customPreparation I6, Step 2
2. customquenched with sat. NaHCO3
3. extractionextracted with EtOAc (2×)
4. washwashed with brine
5. dry with materialdried (sodium sulfate)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification by flash chromatography