تفاعل #304471

ord-31871cbab12347cd824ef51313e43fb6

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGAfter the reaction solution was stirred at room temperature for 30 minutes
  2. 2
    ترشيحthe precipitate was collected by filtration
  3. 3
    غسيلThe precipitate was washed in succession with water and diethyl ether
  4. 4
    أخرىdried under reduced pressure

الإجراء التجريبي

Potassium thioacetate (2.54 g, 22.2 mmol) was added to a suspension of 4-(5-chloro-6-cyano-1H,3H benzo[de]isochromen-6-yl)-6-methylsulfinyl-[1,3,5]triazin-2-ylamine (4.00 g, 11.1 mmol) in N,N-dimethylformamide (100 mL) at room temperature. After the mixture was stirred at room temperature for 6 hours, an 2N aqueous sodium hydroxide solution (100 mL) was added thereto. After the reaction solution was stirred at room temperature for 30 minutes, the pH was adjusted to 5 to 6 with 1N hydrochloric acid. Water (200 mL) was further added to the solution, and the precipitate was collected by filtration. The precipitate was washed in succession with water and diethyl ether, and then dried under reduced pressure. The title compound was obtained as brown solid (3.25 g, 88%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08193351B2uspto-grants-2012_06