تفاعل #2017279

ord-3a9fd2ebc1234ff5bd9ebd61bee4665f

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITwas continued for 1 h
  3. 3
    workup.ADDITIONThe mixture was poured onto ice water
  4. 4
    ترشيحThe precipitate was filtered
  5. 5
    غسيلthe residue washed with water
  6. 6
    تجفيفdried under vacuum over calcium chloride

الإجراء التجريبي

To a solution of berberine hydrochloride (3,718 g, 10 mmol) in pyridine (30 mL) was added portionwise sodium borohydride (450 mg, 12 mmol) and the mixture was stirred at room temperature for 30 min. More sodium borohydride (380 mg, 10 mmol) was added and stirring was continued for 1 h. The reduction was monitored by TLC (DCM-ethyl acetate-methanol 4:4:2). The mixture was poured onto ice water. The precipitate was filtered, the residue washed with water and then dried under vacuum over calcium chloride to give 2.860 g of title compound in about 85 % yield.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08188109B2uspto-grants-2012_05