تفاعل #43266

ord-0773a887e5a640d0900c1ea36d2e3653

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe methanol is removed under reduced pressure
  2. 2
    workup.ADDITIONthe reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid
  3. 3
    استخلاصThe mixture is extracted three times with in each case 100 ml of ethyl acetate
  4. 4
    تجفيفThe combined organic phases are dried over MgSO4
  5. 5
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

2.0 g of ethyl 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionate are suspended in 100 ml of methanol, and 32.1 ml of a 2M NaOH solution are added. The reaction mixture is stirred at 80° C. for one hour. The methanol is removed under reduced pressure and the reaction mixture is adjusted to pH 4 by addition of concentrated hydrochloric acid. The mixture is extracted three times with in each case 100 ml of ethyl acetate. The combined organic phases are dried over MgSO4 and then concentrated under reduced pressure. This gives 1.85 g of 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-3-(tetrahydropyran-4-yl)propionic acid as a solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07732440B2uspto-grants-2010_06