反应详情

A solution of 15.0 g of 1-(2-benzamidophenyl)indoline of Example 19, and 45 ml of phosphorus oxychloride is refluxed under N2 for 4 hours and then the excess reagent is removed to leave a syrup which is dissolved in absolute ethanol, boiled one hour, then concentrated again to a dark purple syrup which eventually solidifies affter prolonged standing. This material is slurried in absolute ethanol, and treated dropwise with enough Bu3N to change the color from purple to orange-brown, whereupon the product base crystallizes voluminously. After refrigeration overnight, the resultant orange-brown flakes are collected, washed with ethanol and hexane, and dried to afford 1,2-dihydro-6-phenylindolo[1,7-ab][1,5]benzodiazepine, m.p.141°-143° C.

1. customthe excess reagent is removed
2. customto leave a syrup which
3. concentrationconcentrated again to a dark purple syrup which
4. additiontreated dropwise with enough Bu3N
5. customcrystallizes voluminously
6. waitAfter refrigeration overnight
7. customthe resultant orange-brown flakes are collected
8. washwashed with ethanol and hexane
9. customdried