تفاعل #540315

ord-b5136db6a79942b4b13e67d73b72557e

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed with water (50 mL)
  2. 2
    أخرىThe organic layer is separated
  3. 3
    تجفيفdried over anhydrous Na2SO4
  4. 4
    ترشيحfiltered
  5. 5
    تركيزconcentrated
  6. 6
    أخرىThe residue is then separated via FCC (EtOAc/heptanes 1:9 to EtOAc/heptanes 1:1)

الإجراء التجريبي

Example 7-A, 5-trifluoromethyl-pyridin-3-ylamine, (385 mg, 2.37 mmol) is taken up in THF (25 mL) and pyridine (0.38 mL, 4.75 mmol) at 0° C. before phenyl chloroformate (558 mg, 3.56 mmol) is added. After 2 h, the reaction is diluted with DCM (50 mL) and washed with water (50 mL). The organic layer is separated, dried over anhydrous Na2SO4, filtered and concentrated. The residue is then separated via FCC (EtOAc/heptanes 1:9 to EtOAc/heptanes 1:1) to give the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08492393B2uspto-grants-2013_07