반응 #76682
ord-024ce929433f44509d6cf287f724db6b
반응 방정식
시약
없음
반응 조건
온도
130°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도was heated
- 2온도The reaction mixture was cooled
- 3온도which was further heated
- 4온도to reflux at 130° C. for 2 hours
- 5기타The residue obtained
- 6workup.DISTILLATIONby distilling off the solvent under reduced pressure
- 7기타was purified by silica gel chromatography (hexane:ethyl acetate=2:1)
실험 절차
A mixture of 2-amino-3-cyanofuran (270 mg, 2.5 mmol), triethyl orthoformate (1.5 ml, 9.0 mmol), and acetic anhydride (0.18 ml, 1.9 mmol) was heated to reflux at 130° C. for 2 hours. The reaction mixture was cooled, and 2-aminoindan (670 mg, 5.0 mmol), sodium acetate (640 mg, 7.8 mmol), and acetic acid (1.1 ml, 19 mmol) were added, which was further heated to reflux at 130° C. for 2 hours. The residue obtained by distilling off the solvent under reduced pressure was purified by silica gel chromatography (hexane:ethyl acetate=2:1) to obtain the title compound (44 mg, 0.18 mmol) having the following physical properties: