反应详情

To a suspension of 6,7,8,9-tetrahydro-5H-1,4,10a-triaza-cyclohepta[f]inden-10-ol (5 g, 29.4 mmol) in toluene (20 mL) was added phosphorus oxychloride (37 g, 246 mmol) and diisopropylethylamine (3.1 g, 24.6 mmol). The mixture was heated to reflux for 40 min then cooled to room temperature. The product crystallized from the reaction mixture on standing over a two-day period at room temperature. The solid was collected and washed with ether to give 10-chloro-6,7,8,9-tetrahydro-5H-1,4,10a-triaza-cyclohepta[f]indene (2.3 g, 42.5% yield). The product was used without further purification.

1. temperatureThe mixture was heated
2. temperatureto reflux for 40 min
3. customThe product crystallized from the reaction mixture
4. waiton standing over a two-day period at room temperature
5. customThe solid was collected
6. washwashed with ether