反应详情

A solution of 10.0 g (9.7 g corrected for 97% purity) of hydroxylamine-O-sulfonic acid (HOSA) in 35.9 g of N-methylpyrrolidinone (NMP) is prepared and chilled to 0–5° C. A second solution is prepared from 20.3 g (19.3 g corrected for 95% purity) of potassium tert-butoxide and 35.3 g of NMP. An amination vessel is charged with 7.0 g (6.7 g corrected for 99% purity) of carbazole, 21.7 g of NMP and an initial charge of 1.3 g of the potassium tert-butoxide/NMP solution. The HOSA/NMP solution and the remaining potassium tert-butoxide/NMP solution are then simultaneously and proportionally metered into the amination vessel over a period of 86 minutes while maintaining a reaction temperature of 22–30° C. to yield a solution containing an 85% yield of 1H-carbazol-1-amine as determined by HPLC.

1. temperaturechilled to 0–5° C
2. temperaturewhile maintaining a reaction temperature of 22–30° C.
3. customto yield a solution