تفاعل #40668

ord-5b1739874cf74cd0a4adf4f3312b5832

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux for 2.5 h
  2. 2
    ترشيحThe reaction mixture was filtered through a cake of Celite®
  3. 3
    غسيلwashed the cake with CH2Cl2
  4. 4
    أخرىThe solvent was evaporated under reduced pressure
  5. 5
    أخرىThe desired product was purified by column chromatography
  6. 6
    أخرىover 60 min
  7. 7
    غسيلas eluting gradient

الإجراء التجريبي

To a solution of 2e (40 mg, 0.168 mmol) in CH2Cl2 was added benzoyl isothiocyanate (30 mg, 0.189 mmol). The reaction mixture was kept at reflux for 2.5 h. The reaction mixture was filtered through a cake of Celite® and washed the cake with CH2Cl2. The solvent was evaporated under reduced pressure. The desired product was purified by column chromatography using 0 to 80% EtOAc in hexane over 60 min as eluting gradient to afford 2f (76 mg, 99%) as a powder. MS (ES) m/z 402 [M+H]+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728008B2uspto-grants-2010_06