تفاعل #53800

ord-f878aee7251846608a61d35112572504

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe tetrahydrofuran was removed on the rotary evaporator
  2. 2
    أخرىto give a solid
  3. 3
    أخرىThe solid was triturated with hexanes/ethyl acetate, 1/1, v/v
  4. 4
    أخرىwas triturated a second time with hexanes/ethyl acetate, 4/1, v/v

الإجراء التجريبي

The product from Example 3, 5-(5,6-difluoro-1H-indol-2-yl)-2-methoxy-phenylamine (0.277 g, 1.0 mmol) was mixed with 3-isothiocyanatopyridine (0.146 g, 1.07 mmol) in tetrahydrofuran (10 mL) and was heated briefly to 50° C. and then allowed to stand overnight at room temperature. The tetrahydrofuran was removed on the rotary evaporator to give a solid. The solid was triturated with hexanes/ethyl acetate, 1/1, v/v and was triturated a second time with hexanes/ethyl acetate, 4/1, v/v to give the product (0.309 g), mp 128-130° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858739B2uspto-grants-2005_02