تفاعل #69446

ord-cf98abd219ca4358bf00f074d9ea0fbf

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvents were evaporated
  2. 2
    أخرىthe residue azeotroped twice with MeCN
  3. 3
    أخرىdried under vacuum at 50° C
  4. 4
    استخلاصThe remaining solid was then extracted with DCM
  5. 5
    تجفيفThe DCM was dried over MgSO4
  6. 6
    تركيزconcentrated

الإجراء التجريبي

Hydrogen chloride (4M in dioxane) (2.4 mL, 9.6 mmol) was added to a stirred solution of tert-butyl 2-(6-(methoxycarbonyl)-2-morpholino-4-oxo-4H-chromen-8-yl)pyrrolidine-1-carboxylate (440 mg, 0.96 mmol) dissolved in dioxane (3 mL) and DCM (3 mL) at room temperature and the reaction mixture stirred for 4 h. The solvents were evaporated and the residue azeotroped twice with MeCN and dried under vacuum at 50° C. The remaining solid was then extracted with DCM. The DCM was dried over MgSO4 and concentrated to afford methyl 2-morpholino-4-oxo-8-(pyrrolidin-2-yl)-4H-chromene-6-carboxylate (286 mg, 83%) as a pale beige solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530470B2uspto-grants-2013_09